UDC 666.2.01

METHODS FOR THE ELECTROPHORETIC SHAPING

OF CERAMIC PRODUCTS FROM AQUEOUS SLIPS

OF INORGANIC MATERIALS (A REVIEW)

E. I. Suzdal’tsev1 and D. V. Kharitonov1

Translated from Ogneupory i Tekhnicheskaya Keramika, No. 9, pp. 16 – 25, September, 2003.

An overview of the state-of-the-art in the use of technologies for electrophoretic shaping of ceramic materialsfrom aqueous slips of inorganic materials is presented and a critical analysis of both strengths and limitationsis given. The need for more efforts in the improved production of large-sized preforms with irregular profileusing advanced electrophoretic deposition techniques is emphasized.

The electrophoretic shaping of ceramic components —in our opinion, an advanced technique that allows, in particu-lar, a high rate of mass buildup during the formation of a pre-form — has been given insufficient attention in recent years.The studies in this field, even popular, are desultory and failto provide an overall picture. Therefore our goal in this workwas a generalization and analysis of available literature dataconcerned with the electrophoretic shaping of ceramic com-ponents from aqueous slips of inorganic materials.

As has been mentioned in the literature [1, 2], the discov-ery of electrophoresis (the term derives from electro + Greek

phoresis — being carried; transmission) belongs to Reus, aprofessor at the Moscow University, who, in the early 19thcentury, observed two previously unknown phenomena. Onewas the movement of a liquid (water) contained in aU-shaped tube (which was partitioned with a quartz sand dia-phragm in the lower section) under the action of an externalelectric field: the effect was named electroosmosis. The otherone was the movement of clay particles suspended in a qui-escent liquid under the action of an electric field. This effectis currently known in science as electrophoresis.

Electrophoresis has been extensively studied and hasfound many uses in colloid chemistry, biology, biophysics,medicine, and numerous industries. Thus, electrophoresisjointly with electroosmosis has been used: (i) for determin-ing the fractional composition of gelatins and controllingtheir molecular-mass composition during mixing [3]; (ii) fordosed delivery of drugs directly to inflamed tissues (in par-ticular, deeply seated septic suppurative foci) by an injec-tion-free method [4]; (iii) for treating industrial effluents [5],and (iv) for preparation of ultrapure water [6].

Electrophoresis and electroosmosis effects have foundnumerous uses in various technologies for fabrication of ma-terials and engineering components, for example:

– deposition of inorganic coating on engineering com-

ponents (for example, spreading of ceramic coatings overwire — an operation which can hardly be done by othermethods [7, 8]; deposition of fireproof coatings on cookware[9]; deposition of antifouling coatings on the electrode ofchemical current sources [10, 11]; deposition of special coat-ings on various substrates [12, 13]) — in these operations,the loss of material is reduced to a minimum, and the processcan be readily automated, with stringent control of the coat-ing thickness even for components of irregular shape; depo-sition of biologic glassy ceramic materials on medicinal tita-nium implants to improve the implants’ mechanical strengthand efficiency [14]; precisely localized deposition of brazingmaterial [15];

– preparation of new materials (preparation of transpar-ent films [16 – 18], ceramic fibers [19, 20], ceramics withconical pores [21, 22], superconducting ceramic materials[23], wear-resistant and thermally stable materials [24], pie-zoelectric ceramic components [25], and ceramic multilayercomposite materials [26, 27]);

– dehydration of ceramic suspensions (an electropho-retic dehydration method of clay suspensions was used in theproduction of decorative mosaic tiles [29, 30] which madethe use of batch-operated filter presses unnecessary).

In addition, further works concerned with an interestingapplication of electrophoretic techniques may be quoted,namely, the shaping of ceramic components from the slips ofinorganic materials [2, 31 – 53].

The pioneers in the field were A. S. Berkman and co-workers who conducted, as early as the 1940s, studies on the

Refractories and Industrial Ceramics Vol. 45, No. 1, 2004

421083-4877/03/4501-042$25.00 © 2004 Plenum Publishing Corporation

1 Tekhnologiya Research and Production Enterprise, Obninsk,Kaluga Region, Russia.

molding of porcelain crucibles using the principle of electro-phoresis [33]. Later, in the mid-1950s, Kainarskii and Mali-novskii used electrophoresis as a method for shapingthin-walled porcelain products [34]. In the late 1970s, studieswere conducted that were concerned with the developmentof a technology for electrophoretic shaping of chinaware[35, 36]. Other works concerned with the shaping of pro-ducts from quartz [31, 37 – 39] and shell molds from lithiumaluminosilicate ceramics [40, 41] by electrophoretic deposi-tion may be cited. The use of electrophoretic method for pro-duction of components from alumina [2, 32, 42] and alumi-num nitride [43] was reported. The aforementioned sourcesprovide compelling evidence that electrophoresis can beused as a means of shaping ceramic products using slips ofinorganic materials; furthermore, electrophoretic shaping is asimple and inexpensive technique for preparing ceramics,and it allows ready control of processing parameters and,consequently, the structure of the deposited material [44].

The principle of electrophoretic shaping of ceramic pro-ducts is as follows. The particles that are suspended in a slipstart moving under the action of an electric field (generatedby applying voltage to the electrodes of a mold equipment)towards the electrode that bears an opposite charge to be-come deposited on it; thereby, a body for the preform is built(see Fig. 1). Positive or negative charge can be applied to theshaping electrode (depending on the surface charge of theparticle); usually, the shaping electrode serve as an anodeconsidering that the particles typically carry a negativecharge. The cathodic processes are of minor importance forelectrophoretic deposition, whereas the processes that occuron the anode merit more attention.

Electric current passing through the aqueous slip causeswater electrolysis which is manifested by the release of oxy-gen at the anode, and of hydrogen at the cathode. The re-leased oxygen may behave in two ways. First, it is capable ofreacting with the material of the anode during the entire pro-cess of the preform buildup and thus becomes bound to it.Second, the oxygen can form a protective oxide film whichwill prevent further oxidation of the anode material. The re-leased oxygen, unable to further react with the anode mate-rial, will accumulate at the anode surface. Situations mayarise where oxygen is unable to escape through the contactclearance between the anode surface and preform surface,which will finally lead to the break of accumulated oxygenthrough the deposited material and to impairment of its struc-tural integrity (formation of pits, blisters, or blow-holes).

Therefore, the choice of a proper material for the shapinganode was a major challenge in the pioneering studies ofelectrophoretic deposition. Berkman in his work [38] de-scribed the following experiment: porcelain slip was pouredin a metal mold (an anode) inside which a metal rod (a cath-ode) was positioned; this done, voltage was applied. How-ever, the electrophoretically deposited material stuck to theanode surface, and the end product (the preform), whentaken off the anode, was of poor quality. To remedy the situa-tion, various lubricants were tried, occasionally with good

results [33]; still, most attention was concentrated on appro-priate materials for the anode. Thus, an anode electrodemade of iron was good enough and could be used to preparepreforms with a smooth surface; however, the surface, for allits smoothness, was colored several tints of yellow becauseof the side effects of water electrolysis, mainly associatedwith oxidation. To prevent oxidation, carburized, chromi-um-plated, passivated (treated with strong nitric acid), andcobalt-plated iron electrodes were used. Carburized and pas-sivated electrodes gave poor results because of the reluctanceof oxygen to bind to the electrode surface; likewise, chro-mium-plated electrodes (made of iron, stainless steel, alumi-num, or platinum) gave an uneven, rough surface.

A good effect was obtained using cobalt-plated iron elec-trodes: the preforms had a smooth, untainted surface. Satis-factory results were achieved using nickel and copper for theanode; however, copper imparted some yellow color to thesurface.

Thus, according to Berkman, the faulty surface of thepreform, whatever the electrode material used (oxidizable ornot), is most certainly associated with oxygen produced bywater electrolysis.

The study of Antonevich and Butyleva [45] was likewiseconcerned with the search for materials suited to the electro-phoretic shaping of ceramics. They used an experimentalchamber schematically shown in Fig. 2. It was a frame (1 )made of acrylic plastic fitted with an anode (2 ) and a ca-thode (3 ). Porcelain slip was poured through the hole (4 ),and voltage was applied; after a lapse of time the voltage wasswitched off, the slip remains were drained off, and the de-posited material and the anode material were taken for analy-sis. The anode materials tested were aluminum, iron, copper,zinc, tin, lead, brass, and stainless steel.

Shaped ceramics, poor in quality and amount of materialdeposited, were obtained using anodes of aluminum and

Methods for the Electrophoretic Shaping of Ceramic Products 43

Power source

Fig. 1. Schematic diagram for the electrophoretic shaping of ce-ramics.

stainless steel, most likely of oxide films formed on the an-ode surface, which prevented the binding of oxygen released.

The anode of tin gave a deposit with a rough surface be-cause of the slow oxidation of the anode material.

Using anodes of zinc, lead, copper, brass, and iron madeit possible to prepare deposits with a smooth surface, uni-form in thickness and texture; however, the ceramics ob-tained on brass, copper, and iron were stained with metal ox-ides (the color could not be removed even by annealing).

High-quality ceramics were obtained using anodes madeof zinc and lead.

Good results were obtained using, as the material foranode, porous ceramics metallized with zinc and lead [45, 46],metallized porous plastics, synthetic graphite, or conductingplastics [47]. Still, in our opinion, these materials, because oftheir poor fabricability, are little suited to the production ofshaping electrodes of irregular profile.

Much similar results were obtained by us in our experi-ments using slips prepared from lithium aluminosilicateglass. The best materials for the anode were copper andbrass, which allowed one to prepare preforms with a smoothsurface and uniform density in thickness and height.

The design of a shaping equipment for electrophoreticdeposition is likewise an issue of important concern.

Simplest in design is the unit for shaping ceramic bri-quettes (Fig. 3) which operates on the same principle as de-scribed above [48, 49]. A shortcoming of this design is thatthe slip in the interelectrode space becomes depleted in con-centration with time, which decelerates the shaping.

To resolve the problem, a series of designs has been pro-posed.

A device for leveling off the slip concentration wasworked out in [2] (Fig. 4). A vessel (a bath) accommodates astirrer, a grid counter electrode (cathode), and a shaping elec-trode (anode) positioned symmetrically about the cathodewalls. Slip is poured in the bath, voltage is applied, and thestirrer is allowed to run; the stirrer agitates the slip, and theslip concentration becomes thus leveled off over the entireinterior of the bath, including the interelectrode space. Cau-tion should be exercised to control the stirrer speed to avoidturbulence so as not to cause damage to the surface of thedeposit.

A shortcoming of this scheme is that the slip mixtureneeds to be continuously agitated, and the thickness of pre-forms thus shaped may be insufficient. Furthermore, as theauthors themselves conceded, the device may not be effec-tive enough to provide uniform conditions in the bath; there-fore, an alternative was proposed where the stirrer was re-placed by a membrane pump. Figure 5 shows a sketch of thesetup for shaping ogival and conical hollow bodies of revo-lution.

The setup contains a vessel (a counterelectrode) in whichthe shaping electrode (an ogive) is positioned. The suspen-sion concentration is leveled off as the slip, driven by a mem-brane pump, is allowed to circulate between the vessel and afeed tank.

Using this setup, alumina preforms with a wall thicknessof about 4 mm and a height of up to 40 mm were preparedin [2].

Still, the setup in question is not devoid of shortcomings:It is rather sophisticated in design and provides no way to ob-

44 E. I. Suzdal’tsev and D. V. Kharitonov

SlipShapingelectrode

Counterelectrode

Fig. 3. Schematic diagram of a setup for shaping ceramic products[48, 49].

Stirrer

Cathode

Anode

Fig. 4. Schematic diagram of a setup for levelling off the suspen-sion concentration (after Andrews, Collins, and Cornish [2]).

2

4

3

1Fig. 2. Schematic diagram of anexperimental chamber (after Anto-nevich and Butyleva [45]).

tain thick-walled preforms; furthermore, the electric field po-tential between the electrodes varies with height, which leadsto inhomogeneity in the deposited material. Attempts tomake the electric field more uniform by coating certain areasof the inner surface of the vessel with an insulating varnishcan hardly be, in our opinion, a sufficient remedy.

The problem in question was resolved in [34, 35] wherea technology for manufacture of chinaware was developed.The technology was based on the principle that a uniformelectric field is a necessary condition for depositing layers ofequal thickness; therefore the cathode was shaped in such away that the working surfaces of the two electrodes wereequidistant. The hydrogen-saturated water released duringthe preform buildup moves towards the cathode, then up-wells and spreads over the surface of the slip. To rectify thisdeficiency, a cathode of special design was developed thathad a perforation at slip level to remove water and oxygen.

Using this technology, porcelain cups with a wall thick-ness of 2 – 3 mm could be prepared (with a molding cycle of30 – 60 sec). An attempt to increase the wall thickness to10 – 30 mm may cause a depletion of the slip in the inter-electrode space.

Studies on the electrophoretic shaping of quartz ceramicshave been conducted by a team headed by V. F. Tsarev[37 – 39, 50]. They used a cathode in the form of a perfo-rated metal plate placed on a plaster mold. The cathode holeswere also filled with plaster. The moisture on the outer cath-ode surface was removed via direct contact with a hygro-scopic material (gypsum plaster).

A device was proposed (Fig. 6; [50]) in which the cath-ode was ventilated with air to accelerate the removal ofmoisture; the suspension was fed in under a excess pressure.

Figure 6 shows the operation of the device: The suspen-sion is poured through the inlet tube (1 ); voltage is applied tothe perforated metallic cathode (2 ) (whose perforation holesare filled with a hygroscopic material) and to the anode (3 ).Under the action of an electric field, solid particles move to-wards the anode, and water — towards the cathode to be re-moved as described above.

An advantage of this device is that the concentration ofsuspension is maintained at a constant level during the entiremolding cycle. Another advantage is that the wall thicknessof the preform can be controlled by varying the spacing be-tween electrodes, which allows one to obtain a uniform elec-tric field.

A shortcoming of this method is that fabrication of a per-forated cathode of irregular profile requires an additional andlaborious effort; another inconvenience is the rather sophisti-cated system for ventilating the cathode and creating the ex-cess pressure for feeding the slip.

An attempt was made by the present authors to replacethe perforated cathode with a metallic grid; this modifiedtechnique was good for shaping small-sized preforms but lit-tle suited for preparation of large-sized components with anirregular profile. The main reason for failure was the poorquality of the surface of the plastic mold (it was rough),which prevented easy extraction of the shaped preform with-out damage. To remedy the situation, a modified design wasproposed for preparation of thick-walled preforms(� = 16 – 20 mm) where copper plates were used for the twoelectrodes. Specimens of good quality could be obtained;still, the development of a mold equipment for large-sizecomponents with irregular profile continues to be a challengeto designers, in part, because of the high costs incurred.

A device for the electrophoretic shaping of ceramic pre-forms was proposed [51] based on a porous (plaster) moldwith a metallic electrode (anode) spread over the outer sur-face of the mold and a metallic core (cathode). Electric con-ductivity of the plaster mold was attained by moistening upto a moisture content of 4.8%. Driven by electric current, thesolid particles move towards the anode and become depo-sited on the inner wall of the plaster mold; part of the solidparticles are deposited by osmosis. The hydrogenized water

Methods for the Electrophoretic Shaping of Ceramic Products 45

Vessel

Pump

Slip

Ogive

Fig. 5. Schematic diagram of a setup for shaping ogival and conicalhollow bodies of revolution [2].

Feed

Preformshaped

Air

Slip

1

32

Fig. 6. Schematic diagram of a device for shaping quartz ceramics(after Tsarev and Solomin [50]).

moves towards the cathode to form a layer that preventsfouling.

A shortcoming of this method is that it fails to provide asmooth surface for the reason that, with large-sized preforms,the control of a uniform moisture content in the plaster moldis a difficult task; occasionally, intergrowth of the materialsof shaped preform and plaster mold was observed. Further-more, the water accumulated at the cathode might erode thedeposited ceramic layer, with a detrimental effect on the pre-form’s surface.

Along with the diversity in the selection of proper mate-rials for anode and cathode and the design of electrophoreticdeposition units, various electric-field regimes were consid-ered in the literature. For example, it was proposed in[52, 53] to use a periodic pulse current which might alleg-edly provide a route towards a versatile multiparametric con-trol over the microstructure, composition, and properties ofthe preforms. Still, in our opinion, the increased number ofcontrolled processing parameters may lead to unnecessarytechnological complications under serial production condi-tions, and the use of direct current remains, at least for thepresent, a preferable alternative.

Thus, based on domestic and foreign experience in theuse of electrophoretic deposition for shaping ceramic com-ponents, one comes to the conclusion that at present no effi-cient technique has been developed that would allow themanufacture of large-sized ceramic products, especially ofirregular profile; the problem remains a challenge that willrequire more theoretical and experimental efforts for its suc-cessful solution.

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Methods for the Electrophoretic Shaping of Ceramic Products 47