1. 3 Extrusion molding

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1 1. 3 Extrusion molding 9 Extrusion is a widely used technique, both in the field of traditional and technical ceramics. This method allows the continuous manufacture of products with a constant cross- section. The pieces are cut at the desired length when they come out of the extruder. The weight of extruded parts can vary from a few grams to several tens of kilograms and the wall thicknesses from a few to several centimeters. For instance, extrusion is used for the production of tiles and bricks, refractory materials (bricks, protective tubes, rotating furnace walls, etc.), electric components (insulators, resistors), catalyst supports, heat exchangers and tubes for various applications. The extrusion stage consists of pushing the paste that has been plasticized and previously deaerated through a given geometric die, using a piston or a screw. Piston extruders (Fig. 7-A) work in discontinuous mode and are primarily used on a laboratory scale. The paste is introduced into the chamber, which is then closed again. This chamber can be connected to a vacuum pump to ensure the deaeration of the mixture and heated if necessary. In the case of traditional compositions containing clay, or if a binder in aqueous phase is used (cellulose derivatives), the extrusion is carried out at room temperature and the cohesion of the pieces is ensured by the high viscosity of the paste. When a thermoplastic binder is used (case of technical ceramics), the paste is heated in the chamber during the deaeration/compression phase then extruded. The cohesion of the piece is then ensured by the solidification of the organic phase during cooling. The piston extruder enables extrusion at high pressures and has the advantage of limiting the contacts between the paste and the tools, thus decreasing the risks of pollution. Screw extruders (Fig.7-B) working in continuous mode are used in production. They can treat substantial loads going up to 100 tons per hour. These extruders generally comprise a first feeder chamber into which the paste is introduced in the form of granules, then mixed and deaerated. This mixture is then transported and compressed by one or two feeder screws before being finally extruded through the die. The feeder chamber and the compression screws are maintained at room temperature for traditional and cellulose pastes or heated for thermofusible pastes. The extrusion pressures generally range between 4 and 15 MPa. The frictions generated between the paste and the metal walls of the screw extruders are considerable and can results in the fast wear of the screws as well as a pollution of the paste. The extrusion of hollow profiles is made possible by the use of dies comprising of a central core attached to the die by two or more bridges, called spiders (Fig. 8). The paste is separated as it passes through these bridges and is divided into several flows through the ports.. After extrusion, the pieces leaving the die are cut at the desired length and then placed on suitable supports during the drying and/or debinding stages.

2 10 Fig (7): The two main types of extruders A) piston, B) screw Fig(8): Example of a die for the extrusion of hollow tubes

3 2-dry shaping 2.1- Pressing 11 Pressing consists of a compression of a powder or granules in a rigid matrix (uniaxial pressing) or in a flexible mold (isostatic pressing), so that pressing process involve: powder formation (called granulation for ceramics), die filling, and compaction. Pressing is certainly the most widely used method for shaping ceramic pieces, because it allows the manufacture of relatively complex parts with tight dimensional tolerances and high productivity. A broad range of ceramic pieces is produced thanks to the pressing technique: tiles, plates, refractory materials, abrasives, cutting tools, as well as various electroceramic, magnetic and dielectric pieces. Pressing requires a good flow of the powder and a homogenous filling of the matrix or mold, in order to achieve uniform densities in a reproducible way. Spherical particles with diameter higher than 50 μm exhibit good flow capability. It is therefore necessary to granulate ceramic powders in the form of agglomerates, called granules, in order to confer on them the properties required for pressing. The effectiveness of the compaction process is quantified using the compaction ratio, CR, which is defined as the ratio of the pressed product density to the filled die density (an inverse ratio of volumes also works since the mass stays constant):.. (x) For most ceramic pressing, a CR < 2.0 is desired since it reduces both the punch displacement and the compressed air in the compact. As indicated in Eq.(x), a high fill density leads to a low CR. For comparison, the CR in metal powder pressing is typically much greater than 2.0 due to the ductility of the particles Uniaxial pressing Uniaxial pressing in a metal matrix, with one (single effect) or two (double effect) pressing pistons, is used for the production of pieces whose thicknesses is higher than 0.5 mm, with a high surface/thickness ratio. The The scheme of the die pressing method is presented in fig(9) below:

4 12 Fig (9): The scheme of the die pressing method Compression behavior It is generally believed that the sequence of stages occurring during the pressing of spray-dried powder is as follows: stage I: rearrangement of the granules; stage II: deformation or fragmentation of the granules, elimination of porosity between the granules (intergranular macroporosity); stage III: elimination of the microporosity present initially inside the granules (intragranular microporosity), by rearrangement or fragmentation of the particles. These stages are illustrated in Fig.(10) and Fig.(11):

5 13 Fig (10): Evolution of intergranular and intragranular porosity during the pressing of a spray-dried powder Fig (11): The three stages in pressing The variation in the relative density of the compact, under the action of the applied pressure, therefore results from two generally successive phenomena: the progressive removal of intergranular porosity, followed by a reduction in microporosity, initially present in the granules between the particles that constitute them. Wall effects During uniaxial pressing, a fraction of the applied load is transmitted to the walls of the matrix. The powder/matrix frictional forces lead to pressure gradients and therefore density gradients within the green part. The average axial pressure Ph transmitted at a depth h of the piece can be expressed according to the pressure applied P by:

6 14 where f is the powder/matrix friction coefficient, σ r / a the ratio of the radial stress to axial stress and S f /S p the ratio of the friction surface to the pressing surface. In the case of single effect pressing of a cylindrical piece with thickness e and diameter d, S f /S p = 4e/d. In the case of double effect pressing, the pressing surface is double (S f /S p = 2e/d) and the minimum pressure is located at mid-thickness. highlights that, the longer and narrower a part is along the pressing direction (high e/d), the less dense it will be. Uniaxial pressing is consequently restricted to the realization of pieces with a high surface/thickness ratio. The use of a lubricant, either on the matrix walls, in the spray-drying formulation or by coating of the granules, will provide a better transmission of the pressure by reducing the terms f and σ r / a. The choice of the material and the roughness of the surfaces in contact within the powder are also parameters that must be taken into account. Fig (12) schematizes the pressure profiles within a compressed piece starting from a non-granulated powder, for which particle mobility is low. The density gradients that result will therefore lead to differential shrinkages during sintering ( diabolo effect in single effect pressing). Fig (12): Pressure profiles within a compressed piece starting from a non-granulated powder Springback The elastic energy stored in the green part during compression leads to an expansion of the piece, called springback, at the time of ejection. The springback increases with the pressure and is higher for a pressing temperature below the Tg of the organic phase.

7 15 Flaws The main flaws encountered during pressing are the lamination perpendicular to the pressing direction and the rising of the upper part of the piece in contact with the piston (end capping). They are mainly due to the pressure gradients within the piece, the differential springback between the part outside the matrix and the part still stressed by the matrix during ejection, and the piece/matrix friction. The solutions consist of: i) increasing the ductile behavior of the granules (plasticizer), ii) reducing the piece/matrix friction (lubricant) and iii) increasing the mechanical strength of the green part (binder). 2.2 Isostatic pressing Isostatic pressing is used for the production of pieces that are difficult to obtain by uniaxial pressing: elongated pieces (tubes), with complex shapes and/or large volume (spark plugs, cast metal refractory tubes). This pressing method offers the advantage of leading to a homogenous distribution of the pressure inside the piece and thus is also used to produce pieces requiring a high and very uniform green density (bearing and grinding balls, medical prostheses). The granules are similar to those prepared for uniaxial pressing, but are generally more ductile. A deformable mold (silicone, polyurethane), with the shape of the part to be produced, is filled with the granules. A pressure of about MPa is applied to this flexible envelope via a fluid, generally oil Wet mold pressing (fig 13-a) The filling of the mold is carried out initially. The use of a vibratory table improves the homogenity of the filling. After a vacuum deaeration, the molds are immersed in the fluid contained in the compression chamber and are pressed. This process is reserved for bulky pieces and those with complex shapes Dry mold pressing (fig13-b) The mold is filled here directly in the press. The pressure is applied only radially by a fluid between the deformable mold and a rigid carcass. This process allows a higher output rate than wet mold pressing and is used for the manufacture of small pieces. The important types of isostatic pressing are: Cold isostatic pressing (CIP) is conducted at room temperature hot isostatic pressing(hip) which is a process of applying pressure and heat, where the product have to be sintered under pressure in inert or non-oxidizing atmosphere ( N 2 or argon). Due to applying pressure and heat at same time so the high product density achieved which is higher than sintering and then pressing. The used temperature usually 0.5 T m and used pressure 240 MPa. this method is limited to simple shapes magnetic recording heads, gas turbine fan made from Si 3 N 4.

8 Semi-isostatic pressing Semi-isostatic pressing is a combination of isostatic and uniaxial pressing (Fig. 14). It is widely used for the production of flat pieces like plates and dishes which have a high diameter/thickness ratio with thicknesses lower than 5 mm. A metal punch applies a uniaxial pressure to the simplest surface of the part (hollow part of the plate) and a flexible membrane applies, using a fluid, an isostatic pressure to the other surface of more complex shape. The filling, pressing and extraction carried out simultaneously on revolving tables allow high rates of output. The main advantages compared to shaping by plastic deformation are the elimination of drying and great dimensional accuracy. Fig (13): Principles of isostatic pressing: a) wet mold, b) dry mold Fig (14): Principle of semi-isostatic pressing 2.4 Roller compressing The granulated powder can be continuously compressed between rollers for the production of sheets with thickness of about 1 mm.

9 3. Injection molding 17 The mass production of ceramic pieces by injection molding became widespread first in the field of textiles (thread guides) and electronics (packages) before being used for the design of thermomechanical ceramics (valves, rocker arm shoes) and refractory materials (nozzles). In the field of traditional ceramics, however, the attempts towards the industrialization of this manufacturing technique have been hampered until now by the additional costs for equipment and organic additives, compared to the traditional methods of casting and pressing. The pieces produced are generally limited in size and have a thickness lower than 1 cm, with the notable exception of refractory parts that can have a thickness of 2 to 3 cm. Injection molding consists of filling a mold whose shape is that of the piece to be manufactured by introducing into it under pressure the mixture, called feedstock, previously plasticized. This mixture, generally thermofusible, is heated in a chamber and then forced through a low diameter tube into the mold, whose temperature is lower than the melting point of the mixture. After solidification, the piece is ejected from the mold. The value of the pressure determines two injection techniques: high pressure and low pressure injection molding. The high pressure injection molding process, which is used most often, is directly inspired from the technology of injection molding of plastics. Thermoplastic polymers with high melting point confer on the paste a high viscosity, and high pressures are necessary (between 50 and 300 MPa). The pressure is applied mostly by a screw/piston system (fig 15). The screw, with a suitable profile (pitch, thread height, compression ratio), ensures the plasticization of the mixture (mainly by friction), its transport from the feed hopper to the screw head and its compression at the screw head. This compression makes the screw move back. When the mixture volume necessary for the injection is plasticized and compressed at the screw head, the rotation is stopped and the screw then acts as a piston to inject the mixture into the mold through the feed nozzle. Immediately after the injection phase, the screw maintains a residual pressure often amounting to 50% of the value of the injection pressure (Fig16). In fact, the pressure decreases quickly in the mold because of the shrinkage of the mixture on cooling. It is therefore necessary to apply a residual pressure during cooling in order to provide the additional matter for filling the mold. The temperature of the mixture, higher than the melting point of the binder at the time of injection, is about 100 to 220 C depending on the polymers used. The mold is generally heated to C in order to avoid a too rapid cooling of the external envelope of the injection molded parts in contact with the metal walls. Because of the temperature-sensitivity of polymers and in order to avoid their premature degradation, the injection molding technique requires a strict control of the pressure and temperature cycle. In addition,

10 18 the abrasive nature of ceramics calls for the use of abrasion-resistant materials (surface treatment of the injection screws, cylinders and molds) in order to limit the pollution of the ceramic composition. The cost of the high pressure injection equipment is therefore relatively high and remains a major disadvantage of this technique. Low pressure injection molding (medium or low) calls for the use of binder families different from those used for high pressure injection molding. These binders allow the manufacture of ceramic pieces under less restrictive pressure and temperature conditions. The organic phase mainly consists of paraffins, waxes and other binders with low melting point and low viscosity, such as ethyl-vinyl-acetate (EVA) [KOS 97]. In the case of medium pressure, the parts are obtained by injection molding under a pressure from 1 to 5 MPa applied by a piston (Fig17). In the case of low pressure (0.6 to 0.8 MPa), the mixture is forced into the mold by compressed air (Fig17b). In both cases, the injection temperature does not exceed 130 C and the mold is, or is not, controlled in temperature. Fig( 15 ): Principle of high pressure injection molding

11 19 Fig(16):Typical evolution of the pressure in the injection mold during a manufacturing cycle of a piece

12 20 Fig (17): Operating principle of low pressure injection molding machines: A) medium pressure, B) low pressure This process uses a much less expensive material than high pressure injection molding, because the temperature and pressure conditions are lower and the stresses imposed on the material are less considerable. Its main disadvantage lies in its capacity to develop a composition with sufficiently low viscosity to ensure a good filling of the mold without compromising the mechanical properties of the injection molded piece and during debinding. Regardless of the injection process, the molds can be complex systems comprising many parts and moving pieces. In addition to the parts of the mold defining the external form of the product to be manufactured, a mold also includes ejectors to separate and evacuate the injection molded product as well as the cores used to obtain relatively complex hollow forms.

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