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1 Journal of the Korean Ceramic Society Vol. 45, No. 11, pp. 744~749, The Influence of Polymer on the Early Hydration of OPC Phil-Hwan Park, Myong Shin Song*, and Kyoung Hee Lee** Isokorea Co.,ltd, Suwon , Korea *Department of Chemical Engineering, Kangwon university, Samchuck , Korea **Department of Materials Science and Engineering, Myongji University, Youngin , Korea (Received October 21, 2008; Revised November 11, 2008; Accepted November 12, 2008) p» y s w vy Á *Á ** ( ) g * w ywœw ** w œw ( ; ; ) ABSTRACT The properties of the polymer-modified mortars are influenced by the polymer film, cement hydrates and the combined structure between the organic and inorganic phases. Also, this quality of polymer modified cement strongly depend on weather condition and polymer cement ratio. To overcome this problem, polymer-modified cement were prepared by varying polymer/cement mass ratio (P/ C) with 0~20% and constant water/cement mass ratio of 0.5. The effect of polymer on the hydration of this polymer cement is studied on different polymer cement ratio. The results showed that the polymer cement paste have increased the viscosity in addition the amount of polymer dosage and the polymers is completed resulting in a reduced degree of hydration caused by different ion elution amount. Also we know that the reactants is calcium acetate as a results of chemical reaction between acetate group in EVA which is hydrolysis in water and Ca ion during hydration of cement. KeyG words : Polymer cement, Polymer film, Cement hydration 1. s q, en, ü, w w w w» w p k ù g j p š. w p 1) l s r š w š s ƒ. w s p 2) w p» p,, ü t,, ü w, ü j š š. w s p 3-7) ƒ ƒw wš, {, ƒw š š š8,9) D.A.Silva 10) w s p ƒ ƒw œ» ƒw p y x šw. w 11) s p ƒ Corresponding author : Phil-Hwan Park Tel : Fax : ƒw r p ƒ ƒwš œ» ƒw w š, p y û, p s p ƒ ƒw w ƒ û p y w. {, ƒw s p w» y w ƒ šw. ü 1990» l v, gj p k, k w» w. p s w k p k PVA w ƒ EVA w» w. s p w s ù, š y ƒ w ü y w w š.»z ù œ gj p,,, x t ¾ w wš. s 744

2 p» y s w 745 Table 1. Chemical Composition of OPC (w%) SiO 2 Al 2 O 3 CaO MgO Fe 2 O 3 Na 2 O K 2 O SO 3 Cl p t w,» y j w e œx œ w j w œ w ƒ. s p k ù gj p šd ƒ, ü», ey, yk, w z. w s p w š» e e wš. w w PC, GRC, CRC, q t y w wš ù t w š. s p w s p ƒ ƒw p» y w w m w. 2. x sp p w.» x sp p y d w Ca d sp p 30, 1, 13, 24 w. s ƒ y Ca d w, ƒƒ w FT-IR, SEM XRD w p x p H sp p w š yw p Table 1, Table s s r xk t, s p ƒ w w, Tg w ü š EVA(Ethylene Vinyl Acetate) y x s ( w s t») w š p Table x yw KS F 2476( x s p k ) w sp p» P/C 0~20%, W/C 0.5 w yww. 20 o C ü s p (%) yw» 2 w, yww w yw 1 30 yww 1 30»w 1 30 yww d x 23±0.5 o C, 50±5% w p s P/C Ratio(%) 0~20% wš W/C 0.5 w 3 z z (Brookfield RVDV II+, 100 rpm, spindle No. 6) w d w. s 50% šx w s r k w d w y d y» KYOWA 10 Data Logger UCAM-60B l w d w, W/C 0.5 w Ca x y Ca d w 2g w 100 ml(w/c =0.5) ƒv j š sw xk k. ƒ d w w 1 mw w e( v l) w w ICP d w FT-IR, wš û e m y g z powder X- z w, y w» w x x ww. w Fourier-Transform Infrared Spectrometer w p y s w k y w. Table 2. Physical Properties of OPC specific gravity Blain (cm 2 /g) ,412 Setting Time (min) Compressive Strength (N/mm 2 ) initial final 3d 7d 28d Table 3. Description of Redispersible Powder Polymer type of polymer ph (20 o C) EVA 8-9 particle size (µm) powder Max.2% >400 after absorbing bulk density (g/l) M.F.F.T ( o C) ± «11y(2008)

3 746 vyá Á Fig. 1. Viscosities of OPC with EVA powder polymer. 3. š 3.1. d Fig. 1 s p y ùkü. 50% šx k s ƒ 2,770 cps p 510 cps w ƒ, s ƒ ƒw ƒ ƒw ùkû. p yy s r m 10 nm ~10 µm j» g w. g w ³ew p. s p yww 0.05~5 µm j» s ƒ 17 µm j» p ³ w ƒw. ƒ w ü w ùkü s yww p r p s ƒ x ƒ ƒw. y w ƒ y p Fig. 2 s p y p ùk ü. OPC s ƒ ƒw y, ùkû. s ƒ q Ca p Fig. 3 Ca ion p ùkü. w, s ƒ ƒw Ca ùkû y d ew š w.,» y s ƒ y j, Ca w w.» w 11) s ƒ w ƒ w, w Ca w Fig. 2. Hydration heat of OPC with EVA powder polymer. Fig. 3. Elution properties of Ca ion of OPC with EVA powder polymer. q Figs. 4~6 FT-IR, Table 4 OPC s FT-IR bands ùkü. Fig. 4 OPC w, Fig. 5 w s. w Fig s p ƒ 20% y FT-IR ù kü. FT-IR calcium hydroxide OH group bands 3642 cm 1, C-S-H w 3440~3446 cm 1, sulfate phases band 1116~1118 cm 1, anhydrous calcium w wz

4 p» y s w 747 Table 4. Bands Identification of OPC and EVA Powder Polymer Bands Identification Bands Identification cm group cm group 3640 OH 3696 OH 3402 S-O 3620 CH S-O OH 1426 CO CH 2, CH S-O 1740 C=O 920 Si-O CH 2, CH 3, CO 3 2- Si-O;Al- O;CO C-CH Al-O 1244 C-O 712 CO C-O, OH 660 S-O 1022 C-O, CH Si-O 944 C-C in ester group 522 Si-O;Al-O CO Si-O;Al-O 748 CH2, CO OCO 606 C=O; ester group 540 C=O Fig. 6. FT-IR spectrum of OPC with 20 wt% EVA powder polymer in KBr pellet. silicates bands 920, 526~536, 458~464 cm 1 ùk ù carbonate phasesƒ 1424~1436, 874~ 880, 704~712 cm 1 ùkû. w s EVA s ethyl acetate group y w. ù Fig. 6 p y s ùkù 1558~ 1568 cm 1 bandsƒ ùkû. EVA s y colloid polyvinyl alcohol(pva) w vinyl acetate group swwš, e w ƒ w(saponification). p Ca(OH) 2 Fig. 4. FT-IR spectrum of OPC in KBr pellet. Fig. 5. FT-IR spectrum of EVA powder polymer in KBr pellet. Fig. 7. XRD of Polymer-Cement composite(p/c ratio(%) = 0, 20) 45«11y(2008)

5 박필환 송명신 이경희 748 Fig. 9. Fig. 8. Hydrates of OPC at 24 h. XRD of Polymer-Cement composite(p/c ratio(%)=0, 20) 포화용액 중에 분산되면, acetate anion(ch3coo) 은 시멘 트 중에서 용해되어 나온 Ca 이온과 쉽게 반응하게 된 다. 이 반응에 의해 calcium acetate가 생성된다. Ca +2(CH3COO) Ca(CH3COO) FT-IR 분석 결과 나타난 1558~1568 cm 의 bands는 폴 리머시멘트 페이스트에서 carboxylate anion(-coo )을 나 타낸다. 그러나 1740~1742 cm 의 bands가 존재하는 것 은 가수분해가 완전하지 않은 것을 뜻한다. 따라서 EVA 계 폴리머를 사용한 폴리머시멘트 재료의 수화 지연은 상 온에서, 수용액 중에 acetate anion(ch3coo) 의 생성에 의 한 것이라 판단된다. Figs. 7, 8에 XRD 분석결과를 나타내었다. Fig. 7은 OPC의 수화물 및 OPC에 폴리머 20 wt% 혼입된 수화물 의 XRD 결과이며, Fig. 8은 Fig. 7에서 ettringite 부분만 확인하기 위한 분석결과이다. XRD 결과를 보면 폴리머 를 첨가하지 않은 OPC 경우, 초기에는 Ca(OH) peak가 미약하고, 24시간 경과 후에는 강한 Ca(OH) peak가 생 성되었음을 알수 있다. 또한 Fig. 8의 ettringite 생성에 대 해서도 일반적인 OPC의 경우 24시간까지 ettringite의 생 성이 원활함을 알 수 있다. 그러나 폴리머를 첨가한 시료 의 경우 수화 초기부터 ettringite의 생성이 거의 나타나지 한국세라믹학회지 Fig. 10. SEM of Polymer-Cement composite(p/c ratio,% = 20) 않음을 알 수 있다. 이는 OPC의 경우와는 달리 폴리머가 혼입된 cement의 경우, 폴리머 중의 acetate group에 의해 Ca ion의 소모로 인하여 sulfate 이온이 ettringite 생성에 기여하지 못하게 되고, 따라서 ettringite 결정의 성장이나 핵의 성장을 지연시키기 때문인 것으로 판단된다. Sulfate ion의 잔류는 Fig. 6의 1130 cm bands에서도 확인할 수 있다. Figs. 9, 10에 SEM 분석결과를 나타내었다. Fig. 9는 일반 OPC 수화물의 재령 24시간에서의 SEM 결과이며 Fig. 10 은 OPC에 폴리머 20 wt% 혼입된 재령 24 시간에서의 필 름형성을 보여준 것이다. Fig. 9의 경우 전형적인 OPC 수 화물의 상태를 나타내고 있으며, 폴리머 20 wt% 첨가한 Fig. 10의 경우 폴리머에 의한 필름의 형성모습을 잘 나 타나고 있다. 본 연구 결과, 폴리머시멘트 비가 증가할 수록 점도가 상승하고 Ca ion 외 각종 이온의 용출저하가 폴리머시 멘트 복합계에서 수화를 지연시키는 주 원인이며, 또 다 른 원인으로 EVA의 일부 가수분해로 acetate가 Ca ion 1

6 w calcium acetate w w sulfate ion» w Ca ion w yƒ q. Ca ion wƒ w» w, acetate w w yw ³ v w q. 4. s p EVA s y w OPC» y w w. EVA s y w yƒ, y s p r p w cement paste Ca ion acetate group sulfate ion w Ca ion» q, yw w calcium acetate q. REFERENCES 1. Z. Su, J.A. Larbi and J.M.J.M. Bijen, The Interface between Polymer-modified Cement Paste and Aggregates, Cem. Concr. Res., (1991). 2. Y. Ohama, Polymer-based Admixtures, Cem. Concr. Compos., (1998). 3. Y.Ohama, Properties of Polymer-modified Mortars Using p» y s w 749 Powdered Emulsion, pp , Polymer Concrete: Use, Materials, and Properties, Publication SP-89, American Concrete Institute, Detroit, V.R.Riley, and I. Razl, Polymer Additives for Cement Composites ; A Review, Composites(Guildford), 5 [1] (1974). 5. H. Hashimoti and Y.Ohama, Effect of Curing Methods on Strengths of Polymer-modified Concretes, J. of College of Eng., Nihon Univ., Serise, A., (1978). 6. S.N.Pareek, Y.Ohama, and K.Demura, Adhesion Mechanism of Ordinary Vement Mortar to Mortar Substrates by Polymer Dispersion Coatings, pp , Proceeding of the 6th International Congress on Polymer in Concrete, Beijing, Y.Ohama, K.Demura, and Y.Jo, Adhesion of Epoxy Mordified Mortars without Hardener, pp , 4th Japan International SAMPE Symposium. Tokyo, Y.K. Jo, W.S. Jeon, and Y.S. Soh, An Experiental Study on the Effect of Curing Conditions on Improvement in Strength of Polymer Modified Mortar, Review of Architecture and Building Sci., 14 [3] (1998). 9. Wan-Ki Kim, Development of Polymer Cement Mortar Modified with Redispersible Powder Polymer(in Jpn.), pp , Ph. D. Thesis, Japan University, Japan, D.A. Silva, V.M. John, J.L.D. Ribeiro, and H.R. Roman Pore Size Distribution of Hydrated Cement Pastes Modified with Polymers, Cem. Conc. Res., (2001). 11. P.-H. Park, A Study on the Adhesives Properties of Wood Flooring based on Polymer Cement(in Korean), Review of Architecture and Building Science, 21 [2] (2001). 45«11y(2008)

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