The article presents results of analyses of ceramic slurries made using materials currently tested in this technology, i.e.: colloidal silica (Ludox AM and Ludox SK) as a binder and Al2O3 as the ceramic matrix material. To characterise the binder, the size of colloidal binder particles, the Zeta potential and the binder pH were determined. Rheological properties were studied for slurries whose proportion of the (technologically justified) solid phase amounted to: 73; 74; 75 %. The impact of the solid phase proportion on the thickness of subsequent coats applied to the wax model, the dynamic viscosity and the density was determined. Research also included the impact of the size of matrix grains and the temperature on the above properties

J. Kolczyk

J. Zych

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55METALURGIJA 52 (2013) 1, 55-58J. KOLCZYK, J. ZYCHRHEOLOGICAL PROPERTIES OF CERAMIC SLURRIES WITH COLLOIDAL BINDERS USED IN THE INVESTMENT CASTING TECHNOLOGYReceived – Prispjelo: 2012-02-18Accepted – Prihvaćeno: 2012-07-18Preliminary Note – Prethodno priopćenjeISSN 0543-5846METABK 52(1) 55-58 (2013)UDC – UDK 669.55:71.018.9=111J. Kolczyk, J. Zych, AGH University of Science and Technology, Faculty of Foundry Engineering, Kraków, Poland.The article presents results of analyses of ceramic slurries made using materials currently tested in this technology, i.e.: colloidal silica (Ludox AM and Ludox SK) as a binder and Al2O3 as the ceramic matrix material. To characterise the binder, the size of colloidal binder particles, the Zeta potential and the binder pH were determined. Rheological properties were studied for slurries whose proportion of the (technologically justifi ed) solid phase amounted to: 73; 74; 75 %. The impact of the solid phase proportion on the thickness of subsequent coats applied to the wax model, the dynamic viscosity and the density was determined. Research also included the impact of the size of matrix grains and the temperature on the above properties. Key words: investment casting method, rheological properties, colloid silicate, dynamic viscosityINTRODUCTIONThe investment casting technology is one of the old-est methods, utilised in the machine, transportation (railway, aviation, motorisation) and armaments indus-tries. Presently multilayer moulds forming a certain shell kind are applied in this method. The binder being a component of liquid ceramic moulding sands decides, to a signiﬁ cant degree, on the quality of the produced casting moulds and on the casting quality. In the previous technology, and partially also cur-rently, ethyl silicate has been applied as a binder. Due to its alcoholic character, this binder relatively easily transfers from the sol state into the gel one, providing the proper technological strength of the layer. Alcohols, having a low evaporation temperature and nearly three times smaller than water heat of vaporisation, are fast removed from the layers of the mould being formed.Presently, new regulations of the environment pro-tection were introduced, which are forcing to withdraw ethyl silicate from the technological process and substi-tuting it by the new (water) binder of the new genera-tion – colloidal silica [1, 2]. Changing of the binder, forces also changes in the ceramic materials applied in the new technology. Ce-ramic moulding sands with a binder in a form of col-loidal silica have several different properties than the ones applied up to day. This concerns the properties, which are very important in the moulds production process. These important properties are as follows reo-logical properties including the dynamic and kinematic viscosity, tendency for sedimentation, wettability of wax patterns. All these properties depend on the ceram-ic mixture composition, kind of colloidal silicate, amount of solids in the mixture, temperature, etc. [3, 4]METHODOLOGY AND PERFORMING OF MEASUREMENTSAs the ﬁ rst step of investigations the particle size in a binder was determined by means of the device: Nano-sizer-ZS of the Malvern Instruments Company. This de-vice allows to determine three basic parameters describ-ing particles in a suspension, it means: size, Zeta poten-tial and molecular mass. The particle size measurement is based on the Brownian movement effect and the dy-namic light diffusion technique. The successive stage of investigations constituted viscosity measurements of a binder and ceramic mould-ing sand, which were based on the ﬂ ow curve determi-nation at the increasing and then decreasing shear rate value. Stress values obtained at the decreasing shear rate were accepted for the results analysis. The rotary viscometer RHEOTEST 2 was used in measurements. This device is applied for investigating rheological characteristics of ﬂ uids in a wide ranges of shear rate, shearing stress and dynamic viscosity. The tested ceramic moulding sand (Ludox AM) and the binder (Ludox AM and SK) was placed in the ring-shape crevice in between two coaxial cylinders of the measur-ing system. The outer cylinder was not moving when the inner one (called a spindle), which rotated with a constant angular velocity, was connected with the meas-56  METALURGIJA 52 (2013) 1, 55-58J. KOLCZYK et al.: RHEOLOGICAL PROPERTIES OF CERAMIC SLURRIES WITH COLLOIDAL BINDERS USED...uring shaft by means of the calibrated spring. The meas-uring cylinder was ﬁ lled with the proper amount of ﬂ uid (binders: Ludox AM and SK of 25 cm3, and ceramic sand on the basis of Ludox AM in an amount of 30 cm3) and then connected with the viscometer meas-uring mechanism [5, 6]. Tests were perfor-med at an ambient temperature (app. 22 oC).The micrometric tests of the thickness of the ceram-ic moulding sand layer deposited on the wax pattern were aimed at the determination of the mixture compo-sition inﬂ uence on the formed layers thickness. Mea-surements were carried out for three different fractions of the solid phase, being respectively: 73; 74; 75 %. Three layers of the ceramic mixture were placed on the wax pattern of dimensions: 60 x 60 x 5 mm. After each layer deposition its thickness was measured.BINDING AGENTS PROPERTIESThe simplest classiﬁ cation divides ﬂ uids into the Newtonian and non-Newtonian ﬂ uids. Ceramic ﬂ uidal sands due to their rheological behaviour can be classi-ﬁ ed into non-Newtonian, pseudoplastic ﬂ uids, where viscosity (apparent) decreases when the shear rate in-creases [6, 7].Several factors inﬂ uence dynamic viscosity, among others: mixture and binder temperature, particle size, percentage fraction of a solid phase, etc. [8, 9]. It can be noticed in Figures 1 and 2 that Ludox SK (pH = 4-5) is characterised by larger particles in the binder as com-pared with Ludox AM (pH = 9). Particle sizes have a signi-ﬁ cant inﬂ uence on the binder viscosity, which is conﬁ rmed by the results presented in Figures 3 and 4.Flow curves of the Ludox AM and SK binders are shown in Figure 3. These binders behave as the Bing-ham plastic, otherwise it is non-Neutonian rheostable ﬂ uid, which starts ﬂ owing only when shearing stresses exceed a certain critical value.Tests indicated the Ludox SK binder has a higher dynamic viscosity, being equal 0,007 [Pa·s]. The vis-cosity curves of binders are presented in Figure 4. The viscosity correlates with the particles size in a binder. Thus, on this basis it is possible to infer that occurrence of larger particles in a binder or in a moulding sand ma-trix will cause an increase of its viscosity. RHEOLOGICAL PROPERTIES OF MIXTURESThe comparison of viscosities of suspensions con-taining the same solid phase fractions but of different Al2O3 grain size, allows to notice that the ceramic moulding sand with addition of aluminium oxide of the grain size: dL = 29 µm is characterised by a higher vis-cosity than the sand containing Al2O3 of the grain size: dL = 16,5 µm (Figure 5). The dynamic viscosity was in-creasing along with the solids content increase due to strong particles interactions. Introduction of a higher amount of the solid phase into the moulding sand causes its viscosity increase (Figures 6 and 7). For sands containing 73 % of the solid phase η = 0,110, for 74 % η = 0,254, and for 75 % η = 0,651 [Pa·s]. At the moulds production, the selection of the mix-ture components proportions should enable obtaining the high ﬁ nal strength of the mould.Figure 1 Particle size in the Ludox AM binderFigure 2 Particle size in the Ludox SK binderFigure 3 Binders fl ow curves Ludox: AM and SKFigure 4 Binders viscosity curves Ludox: AM and SK57METALURGIJA 52 (2013) 1, 55-58J. KOLCZYK et al.: RHEOLOGICAL PROPERTIES OF CERAMIC SLURRIES WITH COLLOIDAL BINDERS USED...CERAMIC LAYERS THICKNESSIntroducing into ceramic mixture too small as well as too large solid phase fraction inﬂ uences unfavourably the quality of produced ceramic moulds, which is seen in Figure 8. The inﬂ uence of the solid phase content on the thickness of the layer formed on the wax patterns is presented in Figure 9.When too small fraction of the solid phase is intro-duced into the mixture the wax pattern surface is not equally covered. After three times immersion of the wax pattern in the ceramic moulding sand some wax gaps can be seen (Figure 8 a). The layer is very thin and its average thickness is 0,16 mm. However, when too large fraction of the solid phase is introduced the dy-namic viscosity increases which leads to uneven cover-ing of wax patterns by the ceramic moulding sand. In addition, it causes pellets formation on the surface (Fig-ure 8 b, c). The layer thickness is then 0,35 mm. Layers deposited on wax patterns become more and more thick which can lead to a mould weakening and decreasing its structural strength. The obtained results are the preliminary ones lead-ing to the development of new optimal compositions of ceramic moulding sands applied in the technology, in order to obtain moulds fully suitable for the production process. The basic properties such as: viscosity, solid phase content and pH value were determined for the Lu-dox AM binder. The performed tests allowed to state that the ceramic mixture containing 74 % of the solid phase is optimal in respect of rheological properties and the layer thickness equals: 0,29 mm. The wax pattern is equally covered.CONCLUSIONSAn important feature of the colloidal silica based binder is its long working time, and none self-gelating tendency (contrary to the ethyl silicate based binders), however this binder can change its viscosity. On the ba-sis of the obtained results, it can be stated that the larger matrix grain size the higher moulding sand viscosity. The second essential factor inﬂ uencing rheological properties of the suspension is the solid phase fraction. The analysis of the measurements indicates that along with the solid phase content increase the investigated moulding sand viscosity also increases. This is not fa-Figure 5  Infl uence of Al2O3 grain size on the  ceramic moulding sand viscosity, Al2O3 fraction = 74 %Figure 6  Ceramic moulding sand (on the Ludox AM basis) fl ow curves; infl uence of the solid phase fractionFigure 7  Ceramic moulding sand (on the Ludox AM basis) viscosity curves; infl uence of the solid phase fractionFigure 8  Wax patterns after placing 3 layers of the ceramic moulding sand of various solid phase contentsFigure 9  Infl uence of solid phase fraction in the mixture on the thickness of layers formed on wax patterns58  METALURGIJA 52 (2013) 1, 55-58J. KOLCZYK et al.: RHEOLOGICAL PROPERTIES OF CERAMIC SLURRIES WITH COLLOIDAL BINDERS USED...vourable for the ceramic moulds production. The proper selection of the sand components is important to obtain the high mould strength.When the dynamic velocity of the mixture increases the deposited layers become thicker and thicker. This makes difﬁ cult their drying and can cause moulds crack-ing during that process. Since the ceramic moulding sands dynamic viscosity is one of the most important features deciding on the ceramic moulds quality, it is constantly controlled in the technological process.The study was performed as the “Dean Project 2011”, No. 15.11.170.420REFERENCES[1] A. Karwiński, G. Para, Prace Instytutu Odlewnictwa XL-VIII 1-2 (1998), 145-169.[2] S. Jones, K. Harris, R.J. Brown, Investment Casting Insti-tute. 52nd Technical Conference & Equipment Expo 2004.[3] M. Dziubiński, T. Kiljański, J. Sęk, Podstawy reologii i reometrii płynów, WPŁ 2009.[4] B. Hutera, The effect of solvent content in binder on the nature of surface phenomena taking place in a sand grains–binding material system, WN Akapit 2008.[5] G. Scharam, Ośrodek Wydawnictw Naukowych PAN, Poznań 1998.[6] A. Karwiński, P. Wieliczko, W. Leśniewski, Inżynieria i Aparatura Chemiczna 5 (2006),58-60.[7] H. Sonntag, Koloidy, PWN 1982.[8] P.K. Senapati, D. Panda, Journal of Minerals & Materials Characterization & Engineering 8/3 (2009), 203-221.[9] J. Firouzi, A.A. Youseﬁ , A.E. Langroudi, Iranian Polymer Journal 2/15 (2006), 127-134.Note:  The responsible translator for English language: “ANGOS” Trans-lation Ofﬁ ce, Kraków, Poland.

Rheological properties of ceramic slurries with colloidal binders used in the investment casting technology

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