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Effect of chemical composition of zinc phosphating solution on phosphate

coating properties

Article  in  Egyptian Journal of Chemistry · January 2009

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48
Effect of Chemical Composition of Zinc
Phosphating Solution on Phosphate Coating
Properties

M. A. Zayedu, F.A. Nour El-Dien and Amal I. Hassan.

Chemistry Deptrt nent, Faa.tlty of Science, Cairo University,l 2 6 I 3
Giza, and'Helwan Engineering Industrial Company, Cairo,
Egypt.

D HOSPIIATE coatingshave a wide field of applicationsin industry.

.f The applications of coatings are classified according to the film
tl,ickiiess ai-rrj i!-re iype of soiution employed. in ihis siudy ihe
phosphating process in the zinc-phosphating-nitrate accelerator on
steel gave a phosphating layer of suitable morphology which was
investigatedby different instrumentslike SEMIEDS and XRD. The
crystal size and the thicknessof phosphatinglayer were found to be
iron content dependent.Therefore, adjusting of phosphate,zinc and
iron concentrationsis very important to get a suitable phosphating
effectivc process. The aim of the present work is to control the iron
concentration in the phosphating bath in order to improve the quality
and adhesive properties of zinc phosphating coating on ste€l sheets
that always used for military purposes in Helwan Engineering
Company in EgYPt-

Keyrvords: Phosphatecoating process.Crystallinity and morphology

of phosphatinglayers,SEM/EDS & XRD measurements.

(r)
Phosphating is the most widely used operation in metal surface pretreatment
process and finishing of ferrous and nonferrous metal. The phosphating process
economy, speed of operation and abiliry to afford excellent corrosion resistance,
@'3).
*"u. ,"ri.tunce. adheiion and lubricatingpropertieswere studied
(t't)
Severalmethods haue been carried out for studying phosphatingsolution
bath composition and its effect on the different propertiesof the formed layer on
met4l surface.It had been shown that the introductionof small quantitiesof iron
into the zinc phosphate bath was beneficial. It decreasedporosity and increased
corrosion resistance; however, the effect was reversed, as the percentageOf iron
in the coating increased(6).
(7)
A process for conffolling the layer weight during phosphating of steel; strip
zinc was coatedon one or both sidesusing soiutioncontainingI to 6 g/l Zn2* ;10 -
30 g/LPO43'.The Fe (ll) ion content within the range of 3 to 100 mg /l was
established in the phosphating solution. lt was found that the higher the Fe (II)

*'f hc correspo 5676624,002-0| 45776675'

ndi ng author:002-02-3
e-mail: rnazir)'cd429(r)vahoo.com
700 M. A.Zayedetal .

content is, the lower the layer weight. An alteration in Fe (lI) concentration from 3
to 20 mgl I gave a change in the layer weight of about 0. I g / m2. The concentration
of Fe (ll) in the rangeof 3-100 mg /l was also usedby Riesopet al.$) and the same
result was obtained. Ferrous ion was also found to affect the phosphating layer on
afuminum strips and its rangehad to be about4-30 mg/l or 10-25gl dependingon
the other constituentslike POes',NHa*, Ni2*, Mn2n,NO3', andZn2* (e).

A method applied manganesephosphatelayer to iron or steel surface was

performed using phosphatingsolution with iron (lI) content0.2-4 gl in presence
of Mn (ll) 10-25gll and 25-50 g/lor 3-35 g/lPO43-('o).Th. effectsof other ions
(rl)
were also studied. Yang et a/. showed that the content af Znz* affects the
('2)
thicknessand integrality of the phosphatingfilm. Also, the pH value and acid
ratio TA / FA, which is defined as the ratio between the total acid (TA) and the
t')
free acid (FR; it:' , were found to have an importantet-iecton the controiiing of
the phosphating processas well as on the rate of nitric acceleratorreaction.

Nicephoroset al.osi found that iron phosphatingsolutionswithout accelerator

gave excellent quality coating on cold rolled and galvanized steel substrates
forming adhesion of subsequentpaint and similar coating, when the solutions
contain at least0.01 g/l of dissolvedanionic titanium. The constituentsof the bath
not only affect the physical propertiesofthe coating layer but they also affect and
(16)
solve the operational problems such as scale and sludge formation. These
problemscan be solved by using compositioncontainingzinc and at leastone of
Ni, Co. or Zn and maintaining an effective level of dissolved iron cation in such
composition.

Experimental
Materials and solutions
All chemicals used were of the highest purity from Merck and BDH. The
water used was twice distilled from all glass.e_guipment.
A concentratedstock
("'
solution of laboratory zinc-phosphating bath was prepared by addition of
142.0ml 67% HNO3 and 380 ml75o/oH3PO4to 160 gZnO, stirring till complete
dissolutionthen 3.3 g Na:PO,r.l2H2Owas addedand diluted to exact one liter in a
measuring flask. Laboratory zinc-phosphatingbath (6 liters) was prepared by
dilution of 75 ml of stock solution. Free acid (FA) and total acid (TA) were
(6)
determined by titrating 10 ml of the bath sample sotution against0. lN NaOH
using methyl orangeand phenolphthaleinindicators,respeetively.

Equipments
The classical volumetric titration methods were performed with micro
burettes,conical flasks and other glassware.

A glass electrode(Orion- ResearchIncorporatedCambridgeMiss. USA) was

utilized to measure and adjust the solutions pH values with the help of ion
analyzerdigital, model 420 A. This electrodewas normally calibratedevery week
by using buffer solutionsof pH values4, 7 and9.

Egltpt.J. Chem.52.No. 5 (2009)

 Effectof ChemicalComposition
of Zinc Phosphating
Solution ?01

Poly Vac Hilger Analyticat Quanta meter model 983 (UK) was used as
instrument for analysis of steel sheets using argon as an inlet gas in Helwan
EngineeringIndustrial Company (HEIC).

A Philips ScanningElectron Microscope(SEM), Model XL 30 attachedwith

energy dispersive spectroscopy(EDS) was used to obtain a microscopic picture
and complete analysis for the zinc-phosphating layer formed on steel sheets.

A Philips X-ray Diffraction (XRD) equipmentmodel PWl7l0 with Ni- filter,

Cu-radiation (), :1.542 Ao) at 40kV, 30 MA and scanningspeed 0.02l sec was
used.

The flame atomic absorption spectrometer PYE UNICAM SP-1900

instrument was utilized fcr the deterrninationof constituentsof bath semples,
especiallyzinc and iron ions.

Fischer coating thickness measurementinstrument for Data-Scope MPIC,

Germany was used to detect the coating thickness of zinc-phosphatelayer
formed.

Procedures
Preparation of samples
Steel sheets; l8- Steel sheetswere phosphatizedin the bath with dimension
( 1 0 c m x l 0 c m x 1 . 0 c m ) o f c h e m i c a l c o m p o s i t i o( C
n : 0 . 1 5 8 % ,S : 0 . 0 0 2 % ,M n :
0.565 %,P: 0.013%o,Si: C.A21Yo and Ni : 0.05%).tingprocessas a standard

Pretreatment and zinc-phosphating process I The steel sheetswere pretreated

before phosphatingusing degreasingsolution (70 gll tri-sodium phosphate,l5 g
sodium hydroxide and 45 g Na2CO3in one liter), pickling by l% HCI solution at
60 "C and 1.0 7o oxalic acid then phosphatizedin the preparedphosphatebath at
60-70 'C for 20 min. After each treatmentthe sheetswere rinsed bv bi-distilled
water.

Collection of samples ; In a first step one sample of the bath was collected
and analyzedfor its constituentsas a standardbefore phosphatingprocess. Six-
sampleswere taken after addition of 0.7 Yo steel chips to the bath, six samples
solutions(Ar-Ao) were collectedafter immersingsix steelsheetsin the bath at 60-
70oC for 20 min. The six sampleswere taken: A1, A2 from different corners of the
bath, A3 from the surface in the center position, Ac, As and 4,6 from different
depths far from the center surface of bath. This process was repeated two times
and symbolized B and C using in eachcaseanothersix steel sheets.81-6and C1-6
samples were taken from the-same positions used before. The concentration of
componentsZn, Fe, and POa'- ions were determinedas the averagevalues for
each step. Finally, the phosphatedsteel sheets were examined for the layers
formed on their surfacesas previouslymentioned.

Egyi:t..|. Chem.52, No. 5 (2009)

702 M. A. Zayedetal .

The testing ofphosphate coatings

The following tests were carried out to ensurethat the zinc phosphatelayers
were formed on the three steel sheetsimmersed in one bath of varied constituents,
and to observe the difference in their properties as a result of the sequenceof
immersion of these sheets.

Examination of appearancerFingernail scratchtest (r8)is a simple appearance

test for crystalline phosphate coatings a white scratch that appearson the surface
without causing injury to the coating to the naked eye is a criteria for good
coatings.

Microscopic examination : These examinations were performed using

scanning electron microscope (SEMy applying energy dispersive spectrcscopic
(EDS) analysis. These examinations were canied out on three different steel
sheetsphosphatedin the bath with varied constituentsdue to the sequenceof
immersionof the sheetin the bath.

X-ray di/fraction (XRD).' X- ray diffraction analysis was carried out to obtain
the type of crystalsthat were formed on phosphatedsteel sheets.The device was
computerizedin such a way that all information (20-intensityand d- spacing)was
produced onto the cornputer print sheet.The d-values obtained arrd their relative
intensity were compared with the data shown by JCPDS cards as a reference.

Determination of coating weight (g/*') t The most important parameter of

phosphate coating is its coating weight per unit area usually expressed in g/m2.
Using a tested sample of phosphatedmetal, the phosphate was chemicaliy
dissoived and coating weight determined by weighing before and after the
(u).
operation The tested piece whose surface area (A) has been determined as
precisely as possible, was weighted (wr). The phosphate was then stripped with
(12% sodium salt of EDTA, 4o/otri-ethanolamine, 9% NaOH and 75Vo H2O)
solution at 70'C for 5 min till constant weight (w). After rinsing with water and
then acetone,the weight loss Sw = wr -w2. Phosphatecoating weight m A in
g/m'was then obtained from the equation:

mA = Sw/A (d^'\

Results and Discussion

Measurements of zinc phosphate coating properties

Many factors usually affect the properties of the zinc phosphatecoat such as
accelerators, solution composition, operating conditions, method of application,
some additives, surface pre-treatment and post treatment after phosphating
process. This research concentrates on one factor, which is the effect of
phosphating batlr composition. The other factors must be fixed during the
process, so that the effect of any change on the physical properties of steel
coating layers only related to the difference in the bath composition. The time of

Egtpt.J. Chem.52,No. 5 (2009)

 Solution
Effectof ChemicalCompositionof Zinc Phosphating 703

irnmersionof the steel sheet was chosento be 20 min at 70 "C. The number of
steel sheets(of dimentionslO x l0 x 1.0 cm) was chosento be six; phosphatedin
a bath of 6.liters capaciry. These conditions lead to the formation of good layer.
This process accompanied by an appreciable decreasein zinc and phosphate as
main components of the bath, and an appreciable increase in the iron content;
which appears due to the dissolution of the iron sheet surface. This process also
gives a chance to study the physical properties ofthe fonned phosphate layer at
different compositions. In case of the actual bath, the conditions are different
oC and the volume
where the time of immersion is 5.0 min, the temperatureis 60
of the bath is large with respectto the surfacearea of the used articles, so the
changein the compositionappearsthroughfew days.

Crystal type of the layer formed is affected by the methods of application

and in oiir procediires we used the immersion iechnique, which gave us a cirance
for studying the change ofbath composition during the process.The surface pre-
treatment of the steel sheets was carried out by two sequencesteps, which were
degreasingand pickling processes,respectively.The post- treatment was water
rinsing and no organic or inorganicadditiveswere addedto the bath.

Morphology, crystal size, coating analysis, crystal type, coating weight and
coating thickness were examined to study the relation between the physical
properties of zinc phosphate layers formed and the composition of the
phosphatingbath.

Table 1 shows the rr€orr.rr€lnertsof crystal size (pm), coating thickness(pm)

and coating weight (g/m2) of three sheetsthat were immersed in phosphating bath
of varied constituents; PO43-,Zn(II) and iron ions , also total acidity (TA) and free
acidity (FT) which differ due to the sequenceimmersion of the steel sheetsin the
bath. The data show that the grain-crystal size decreasesfrom (19 - 42 pm) to
(6-11pm) with the decreaseof POa'-, Zn(II) ion , TA , FA and increase of iron
ion concentration. The crystal size obtained from the SEM micrographs is shown
in Fig.l. The scanning electron micrographs show that the grain crystal size
decreasesas the iron concentration increasesin the phosphating bath. Figure lA
shows a big crystal size (19-42 pm) which formed when the sheet immersed in :'ii:
phosphatingbath containing 200 ppm iron ion, where Fig. lB shows a medium
crystal size (12.6-12.7 pm) when the sheet immersed in phosphating bath
containing 476 ppm iron ion and finally in 861 ppm iron ion concentation the
crystal size (Fig. lC) formed is of small size (6.85 - ll.4 pm). These results
clearly indicate that as iron increasesin the bath a more densely packed granular
crystal with a high degree of uniformity are formed, which create a surface with
greatly increasedsurfaceareathan the underlyingsteel.This phenomenonassists
the more adhesion of the organic mechanical locking of the coating to the
('o).These
phosphate crystal results matched with that mentioned before by
Roesner et al.$). They suggestedthat the introduction of small quantities of iron
into the zinc-phosphating bath is beneficial that it decreases porosity and
increasescorrosionresistance.

Egypt.J. Chem.52,No. 5 (2009)

?04 M. A. ZaYedetal '
coating
TABLE l. correlation between the measurementsof zinc-phosphate
propertiesand the compositionof the bath solution'

Crystal Coating Coating Steel

ComDostion of the bath'
size thickness weight sheet
ms/ml onm ml"
(Frn) 0rm) (g / m')
PO.r' Zn(ll\ Fe(II)'Fe Free Total
(III) Acitlity
Acidity
t9.0-42.0 6.4-10.9 l0-16.5 A
3 1 . 0 0 7.40 200 r8.0 b)

15.0 55 t2.6-21.7 s.6-7.8 8.4-10.7 B

30.70 6.12 476

5 . 8r 861 13.0 50 6 . 8 5 -1l . 4 3 . l- 4 . 1 4.4-5.8

30.l0

Fig.l.Thescanninge|ectronmicrograptrsofthreestee|sheets:(A)Afterfirst
immersion,ln;nftersecondimmersion,(C)Afterthirdimmersion'

C o a t i n g t h i c k n e s s a n d c o a t i n g w e i g h t d a t a p r o v e d t h e d e p -e n d e n c y o n t h e
from (6.4 f0.9 pm)
concentrat;n of phosphatingbath-comfosition. lt ranged
;il (il:les gl#l to (3.1-4.1pm)a;d (4.4- 5.s g1nr),respectively
with the
a""r"ur. of ph-osphateandzinc ionsconcentrations andwith the increaseof iron
ion in the phosphatingbath. These iesults are matchedwith the
"oncentiation et al.$) iho found that the weight could be
iesuttsobtainedby Riesop "9u!il.g
of iron and the higher the Fe(II) contentthe lower
controlledby the concentiation
the coatingweight.

The energy-dispersive is an attractivetool for qualitative

X-rays spectrometer
(20)'
analysisof pltsphate coatings
coatings
Figure2 showsthe EDSqualitativeX-rayanalysisof zinc-phosphate
Each one
for tliree sheetsimmersedin one bath with varied constituents'
a-ir. n i.rorcopic picture(Fig.l). The relative weight and atomic
";"".p*ol6t" , I w) for the ionstiruentswere given by the instrumentunderthe
;;;;; p, re and zn were existing in the zinc
iurve. rhe data obtainedshow that
ohosohatecoatandthereis no otherelementpresentin the coat.The iron appears
rl* formation of phosphophyllitecrystallinestructureand the
ili;;;
(underiyingmetal)' which, may. interfere due to
fr"."n.. of steel carrier
sheet.After first dippingthe coatings
i"n"trution of x-ray to somcextenitolhe
were.foundtocontain(w%)30.0a%P,2|.25%Feand48.37%Zn.Afterthe
Eg.vpt.J. Clrcnt. 52-No' i (2009)
 Effectof Chemical
Composition Solution., :
of ZincPhosphating 705
secondclipping,the coatingcontains26.1VoP,25.25%Fe and 28.65%Zn,while
after the third dippingthe weight Yovrerefoundto be 33.46yop,22.460/o
Fe and
43.90Yo2n.

Thecrystallinephosphatecoatingsobtainedby immersionof threesteelshee8

in the laboratoryzinc phosphatebathwith variedconstituentswere'examinedby
X-ray diffractionanalysis.Figure3 and rable 2 illustratethe X-ray diffraction
patternwith its characteristic
d- spacingand relativeintensities(I/Io) compared
with datashownby JCPDSfiles.The d-spacing and intensitiesof the diffraction
peaksof thebasemetal(steel), monoclinic phosphophylliteZn2FePOa.4 H2Oand
orthorhombic hopeitezn3(Poa)2.4FI2oarelistedin Table2 for identificationof
thephases .

By comparingthe datawith the JCPDSfiles as a reference. Table2 shows

tfiat the iirtensities (d - spacingai 9.16,4.576,2.955A)
of bothhopeitestructure
andphosphophyllite (d-spacing4.438,8.86,3.383,2.833A; increase
structures
as iron increasesin the bath from 200 ppm to 476 ppm.As iron increasesin the
bathup to 861 ppm the relativeintensitydecreases. Fromthe relativeintensities
datarve can calculatewhat is knorvnby "P ratio" which was studiedby many
(6' l{).
11,611'.15

(:'r ::

'l
L.__:i.,0'_f.i{i. r_?r. .s rp dE r& rs ts 1cn.

Fig.2, EDS analysis of the three steel samples.

Egpt. J. Chem.52,No.5(2009)
706 M. A. Zavedetal .

iBi

t0 i0'
20 20 td

Fig.3. X-ray diffraction pattern for the zinc phosphate layers obtained on three steel
sheetsamPles.

TABLE 2. The X-ray data for zinc-phosphate coatings from the bath with varied
.
constituents
Relative intensity (I/I,)
Steelsamples From JCPDS I!e
20 dA Sample Sample Sample Hopiete Phosphophvliitc Base
A B C metal
9.665 9.160 r2.0 20.3 3.8 55
9.90 8.860 8.0 29.3 4.0 85
16.66 5 . 3 1 0 8.3 9.3 2.3 l7
17.50 5.090 25
18.30 4.85 t9.5 30
19.45 4.576 20.7 22.3 2t.9 )) 20
r9.60 4.438 52.9 68.3 31.9 100
t9.70 4.414 25.0 30.0 35
26.00 3.383 20.0 22.3 l9 60
26.15 3.39r 33.0 47.3 t9.5 40
3t.34 2.855 32.0 39.9 t9.5 100 l0
3t.62 2.833 38.0 30.9 32.0 50
34.21 2.614 t 5.5 27.9 14.0 25
40.45 2.222 6.6 5.3 4.7 4
44.53 2.038 t00 100 100 J 100
44.65 2.026 5.0 20 20
50.00 r.433 3.0 30 l2 30
da :Spacing between adiacent latticeplanes
2 0 : Difliaction angleof X-raY

This ratio is the phosphophyllite/ (phosphophyllite+ Hopeite). They found

that when the value of "P ratio" was high, a high colrosion resistance was
obtainedand the presenceofphosphophyllite in the coat increasesthe adhesionof
paint to the phosphatedsteel sheet.Table 3 shows "P ratio" that calculated for the
three cases. The ratio was calculated with respect to the highest relative
intensitiesof the main d - spacing of both structure(dA : 2.855 A for hopeite
Egtpt.J. Chen.52,lJo.5 (2009)
 Effectof Chemical
Composition Solution
of ZincPhosphating 707
and4.438A for phosphophyllite).
The datashowalsothat the relative"P ratio" is
nearly the sameand amountingbetween62 - 63 7o as the iron increasesin the
bathfrom 200 up to 861ppm.

TABLE 3. P/ (P + H) ratio of zinc-phosphatecoating obtained from X-ray diffraction data .

Crystaltype dA Relative intensity (I / Io)

SampleA SampleB SampleC
(P) 4.438 52 67 31 . 9
(H) 2.855 )z 39 19.5
P/(P+H)x100 62Yo 63% 62 o/o

Conclusion

The hard phosphating layer on the surface of the iron required suitable
conditions. In this research the phosphating process in zinc-phosphating -nitrate
accelerator gave a hard phosphating layer of suitable morpholory. The
morphology of the obtained layer was tested by SEIWEDS and XRD tools. The
crystalline size and crystal type lvere found to be iron content dependent. The
increase of iron content in the bath is important for the layer before paint which
has low coating weight and small crystal size. So, it will be more condensedand
has more surface area that increasesthe adhesion of paints on the steel product.
Theseconclusionslead to know that the analytical follow ofphosphate, zinc and
iron contentsof the bath is very important.

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 Effectof ChemicalCompositionof Zinc Phosphating
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(Receivedlll82009 ;
accepted29ll0l20D)

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Egltpt.J. Chryn.52,No. 5 (2CI9)

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