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1 Jurnal f the Krean Ceramic Sciety Vl. 47, N. 5, pp. 81~86, 010. DOI: /KCERS Prperties f Self-hardened Inrganic Cating in the System Alumina-Silica-Calcium Oxide by the Reactin with Alkalies Chang Seb Jen and Tea Wng Sng Department f Advanced Materials Engineering, Kyungnam University, Changwn , Krea (Received August 16, 010; Revised September, September 8, 010; Accepted September 10, 010) e w ù- e- ye»» y gq p Á k û w œw ( ; 010 9, 9 8 ; ) ABSTRACT Sme basic prperties f inrganic catings hardened by the rm temperature reactin with alkalies were examined. The cating paste was prepared frm the pwders in the system Al O -SiO -CaO using blast furnace slag, fly ash and amrphus ceramic fiber after mixing with a slutin f sdium hydrxide and water glass. The mineralgical and mrphlgical examinatins were perfrmed fr the catings prepared at rm temperature and after heating t 100 C respectively. The binding frce f the cating hardened at rm temperature was caused by the frmatin f fairly dense matrix mainly cmpsed f yelite-cntaining amrphus phase frmed by the reactin between blast furnace slag and alkali slutin. At the temperature, fly ash and ceramic fiber was nt reacted but imbedded in the binding phase, giving the fluidity t the paste and reinfrcing the cating respectively. During heating up t 100 C, instead f a break in the cating, anrthite and gehlenite was crystallized ut by the reactin amng the binding phase and unreacted cmpnents in ternary system. The crystallizatin f these minerals revealed t be a reasn that the cating maintains dense mrphlgy after heating. The maintenance f binding frce after heat treatment is seemed t be als caused by the frmatin f welldispersed fiber-like mineral phase which is riginated frm the shape f the amrphus ceramic fiber used as a raw materials. Key wrds : Geplymer, Cating materials, Inrganic cating, Nn-sintered cating, Heat-resistant cating 1. gj p w (binding phase) p r p ù p yw w p p w CO š wš. w wì p x w 1,) ey» w w ƒ w š 1978 Davidvitsƒ s (Geplymer) š )w ƒ xk š. š ù v 4-8) w ey ƒw» gj p xw». s e C-S-H gel w x k š y w Crrespnding authr : Tea Wng Sng Tel : Fax : ù, e y y w x CaO, SiO, Al O y ¾ sw»š» š w ƒ ƒwš. w y NaOH, KOH Na SiO e ù yw s y w» pù gj p gq ƒ w y e š r p l y w ƒ x t» w v w. s w gq y wš w y, œ q gq w w w z w y gq p w z p y wš w. š, v w Al O -SiO - 81

2 전창섭 송태웅 8 Table 1. Chemical Cmpsitin f Staring Raw Materials Raw material Blast Furnace Slag Fly Ash Ceramic Fiber SiO Chemical Cmpsitin (wt%) CaO FeO SO MgO AlO TiO Fig. 1. XRD pattern f fly ash. Fig.. SEM micrphtgraph f fly ash. Fig.. XRD pattern f ceramic fiber. Fig. 4. SEM micrphtgraph f ceramic fiber. CaO 성분계 분말에 가성소다와 물유리로 만든 알칼리 용액을 혼합하여 무기질 코팅재를 제조한 후 상온에서 형 성된 코팅 막과 이를 진공 분위기에서 100 C까지 가열 한 후의 코팅 막의 광물상과 미세구조를 관찰하였다.. 실 험 원료 본 실험에서 사용한 고로슬래그와 플라이애시는 각각 광양제철과 삼천포화력에서 발생된 것을 사용하였으며 세.1. 한국세라믹학회지 ZrO 10 라믹섬유는 (주)모간에서 생산되고 있는 것을 사용하였다. 원료의 화학조성은 X선 형광분석기(PW 400, Philips, 네 덜란드)를 사용하여 분석하였으며, 그 결과는 Table 1에 나타낸 바와 같다. 고로슬래그의 Blaine 값은 600 cm /g, 비중은.91이었으며 플라이애시는 Blaine 값이 700 cm /g, 비중이.8이었다. 플라이애시와 세라믹섬유의 광물상과 미세구조를 X선 회절분석기(PW 710, Philips, 네덜란드) 와 주사전자현미경(S-400, Hitachi, 일본)으로 관찰한 결 과를 Fig. 1부터 Fig. 4로 나타내었다. 그림에서 보는 바 와 같이 플라이애시는 비정질의 유리와 quartz 및 mullite

3 Table. Mixing Rati f Samples Sample N. Blast Furnace Slag Pwder Cmpsitin (wt%) Fly Ash e w ù- e- ye»» y gq p 8 Ceramic Fiber Liquid Cmpsitin (wt%) NaOH Na SiO 74 6, 5~0 µm j» x š. w 1~5 µm xk. e y y yùp (NaOH) KS ³ (Na SiO nh O) w... x š gq y v w v 9,10) gq ³ w» w ww» x w z k Table š w w. š v e k k attritin mill w ¼ 1mm ü w j»ƒ w yww. y y NaOH 0 wt% š w š yw 74:6 š w (L/P ) 0.65 w š w z yww e yww r p. w r p wì š w. r p w gq 0 cm 0 cm q t 0.5 mm Ì sw xw. wr gq y q œ (VCQ-MF-06091, NICHIMEN, Japan) x 100 C¾ w z ¾ ü gq y w. z gq ü ³ ù x (S-400, Hitachi, Fig. 5. XRD patterns f hardened catings prepared frm sample (a)1, (b), (c), and (d)4. 47«5y(010)

4 전창섭 송태웅 84 일본)에 의한 시료 간 비교로 판정하였고 미세구조와 광 물상의 변화는 주사전자현미경과 X선 회절분석기(PW 710, Philips, 네덜란드)로 관찰하였다.. 실험결과 및 고찰 Table 에 따라 고로슬래그, 플라이애시 및 세라믹섬유 의 혼합분말에 가성소다와 물유리의 혼합용액을 가하여 만든 페이스트는 모두 5시간 이내에 흑연판의 표면에서 경화하여 피막을 형성하였고 이를 실제 분말야금 진공소 결 공정에 적용한 결과 실용상 필요로 하는 충분한 경도 와 부착 강도를 가지는 것이 확인되었으며 5배의 확대경 관찰로는 외관상 전혀 균열이 발견되지 않았다. Fig. 5는 충분히 경화된 코팅의 X선 회절분석 결과를 나타낸 것으로서 XRD pattern이 대체적으로 유사한 형태 를 취하고 있으며 대부분 비정질 상임을 보여주고 있다. 여기서 결정상인 quartz는 앞의 분말원료에서 나타낸 플 라이애시 중의 quartz상이 잔존한 것이며, 플라이애시 함 량이 많은 시료에서 더 크게 나타나는 경향성이 이를 뒷 받침한다. 네 개의 시료에 공통적으로 나타난 또 하나의 결정상은 CaO-SiO -H O계 수화물인 yelite로서 이는 주 로 고로 슬래그가 알칼리 수용액과 반응하여 생성한 것 으로 보인다. 이는 잔존된 quartz의 피크로 보아 플라이애 시는 이 반응에 참여하지 않은 것으로 보이며 실제로 플 라이애시나 세라믹섬유를 따로따로 알칼리 용액과 혼합 한 별도의 실험에서도 yelite 피크는 나타나지 않았기 때 문이다. 한편 경화체의 대체적인 XRD pattern은 세라믹섬 유의 XRD pattern과 유사해보이지만 이보다는 정점이 다 소 높은 각도 쪽으로 이동되어 있는 것이 확인되며, 또한 세라믹섬유의 첨가량은 슬래그에 비해 매우 적은 양이므 로 이러한 XRD pattern의 양상은 슬래그의 알칼리 반응 으로 생성된 비정질 지오폴리머에 소량의 yelite가 잔존 하는 이 계의 결합상 특유의 것이라고 할 수 있을 것이 다. Fig. 6은 역시 충분히 경화된 코팅의 수직방향 파단 면의 미세구조사진을 나타낸 결과로서, 모든 시료에서 세 라믹섬유의 모습이 온전한 형태로 존재하고 있음을 확인 할 수 있다. 이로서 코팅이 충분히 경화되어 적절한 경도 와 강도를 발현하는 시점까지도 비정질의 Al O -SiO 계 물질인 세라믹섬유가 지오폴리머 반응에 참여하지 않고 섬유로서의 기능을 하고 있다는 것을 알 수 있다. 따라서 사진에서 결합상으로 볼 수 있는 치밀하고 균질한 부분 은 슬래그의 알칼리 반응으로 생성된 비정질 상으로서 이 것이 시료의 대부분을 구성함을 알 수 있으며 yelite는 여기에 분산되어 있을 것으로 생각되나 특정한 형태를 보 이지 않고 있다. 한편 세라믹섬유는 코팅 막의 파단면 채 취 시에 발생되는 미세균열을 억제한 모습을 보여줌으로 서 코팅의 기계적 물성에도 큰 보강효과를 나타낼 수 있 한국세라믹학회지 Fig. 6. SEM micrphtgraphs f hardened catings prepared frm sample (a)1, (b), (c), and (d)4. 음을 유추할 수 있다. 한편 이들 파단면 사진에서 구형의 플라이애시나, 플라이애시가 박혀있던 흔적을 발견할 수 있으며 그러한 경향성은 플라이애시의 함량에 비례하는 경향을 보인다. 플라이애시나 그 자국의 존재는 구형인 플라이애시가 세라믹섬유와 마찬가지로 지오폴리머 반응 에 참여하지 않음으로서 페이스트의 유동성을 향상시키 는 본연의 역할을 할 수 있었다고 생각된다. 따라서 모든 시료에서 형성된 코팅의 결합상(binding phase)은 고로슬 래그의 반응에 의한 지오폴리머이며 여기에 플라이애시 와 세라믹섬유가 분산되어 기계적 강도가 보강되고 있다 고 판단할 수 있다. 충분히 경화된 코팅이 부착된 상태로 흑연판을 진공소 결로에서 100 C까지 가열, 냉각한 후 관찰한 결과, 코팅 은 외관상으로는 균열의 발생이나 강도하락이 없이 가열 전과 유사한 형태를 유지하였다. 그러나 절취한 코팅의 XRD pattern은 Fig. 7에 나타낸 바와 같이 열처리 전과는 매우 다른 결과를 보였다. 즉 선명한 특성 피크로 CaOAl O -SiO 계 결정성 광물인 anrthite(caal SiO, CAS )와 gehlenite(ca Al SiO, C AS)가 잘 결정화되어 있는 반면 열처리 전의 코팅에서 존재하던 yelite나 플라이애시 중 에 잔존해있던 quartz의 피크는 사라졌음을 알 수 있다. 이들 광물은 다음과 같이 슬래그에서 기인한 비정질 결 합상과 플라이애시 및 세라믹섬유가 모두 반응하여 생성 된 것이라고 고찰된다. 먼저 본 실험에서 사용한 원료나 이를 가지고 조합한 모든 시료들의 CaO-Al O -SiO 성 분의 조합비와 이 계의 상태도 를 기초로 고찰해보면 비 정질 결합상의 조성에서는 gehlenite와 CaO SiO (C S)가 생성 가능하며 실제로 슬래그만을 가지고 만든 별도 실 험의 시료에서는 gehlenite와 C S가 생성, 공존함이 확인 )

5 알칼리 반응에 의한 알루미나-실리카-산화칼슘계 무기질 자기경화 코팅의 특성 Fig XRD patterns f hardened and heated(100c in vacuum furnace) catings prepared with sample (a)1, (b), (c), and (d)4. 되었다. 그러나 SiO 의 함량이 더 많은 anrthite는 생성될 수 없으므로 anrthite의 피크는 플라이애시나 세라믹섬유 가 반응에 개입되었음을 시사한다고 생각된다. 이 때 SiO 함량이 높은 플라이애시의 혼합량이 상대적으로 적은 시 료에는 gehlenite와 anrthite가 함께 생성되어 있고 상대 적으로 많은 시료에서는 SiO 함량이 더 많은 anrthite만 생성되어 있는 것은 플라이애시가 이들 광물의 생성에 소 모되었음을 뜻하며, 열처리 후 quartz의 피크가 사라진 것 도 이를 뒷받침한다. 나아가 슬래그와 플라이애시만의 혼 합으로는 Al O 성분의 부족으로 시료의 조성점이 wllastnite (CaSiO, CS)의 초정영역에 위치하므로 CS도 함께 생성 되었을 것이지만 anrthite만 생성된 점은 원료 중에서 Al O 함량이 가장 많은 세라믹섬유의 조합에 의해 시료 들의 조성점을 anrthite와 gehlenite의 초정영역 가까이 위 치하도록 한 결과 세라믹섬유까지 반응에 참여하였기 때 문이라고 고찰된다. Fig. 8은 열처리 후의 코팅 표면의 미 세구조사진을 나타낸 것인데, 여기에서 세라믹섬유가 섬 유의 형태는 가지고 있으나 열처리 전의 매끄럽던 표면 이 거칠게 변한 것은 이와 같은 결정화 반응때문인 것으 로 보인다. 그러나 정량적인 반응이라고는 말할 수 없고 Fig. 8. SEM micrphtgraphs f hardened and heated(100c in vacuum furnace) catings prepared with sample (a)1, (b), (c), and (d)4. 어느 정도의 깊이까지는 결정화 가 일어났을 것으로 사 제 47 권 제 5호(010)

6 86 Á k. t e w» w ù w gq w» gq ƒ 100 C¾ ü ƒ š. w w gq w ¼ ³ y w ³, w s v anrthiteù gehlenite w gq x»w, xkƒ y z ³ z ƒ. w gq ƒ w yelite w w w ³»». 4. š v ƒw z ƒ yw g ywš 100 C¾ ü ƒ s g q w. y gq w š e yelite w e w» x» v e w š w ƒƒ r p y, gq ³ w» w. 100 C¾ ƒ gq q w v ƒ wì w anrthite ywš gehlenite wì yw e xk» z w gq w ü. Acknwledgment 009w w» û w ü w w. REFERENCES 1. L. Daniel, Y. Kng, and J. G. Sanjayan, Damage Behavir f Geplymer Cmpsites Expsed t Elevated Temperatures, Cem. Cncr. Cmps., 0 [10] (008).. J. Davidvits, Glbal Warming Impact n the Cement and Aggregates Industries, Wrld Resurces Rev., 6 [] 6-78 (199).. J. Davidvits, Geplymer Cement t Minimise Carbndixide Greenhuse- warming, Ceram. Trans., (199). 4. J. Davidvits, Geplymer: Man-made Rck Ge-synthesis and the Resulting Develpment f Very Early High Strength Cement, J. Mater. Educatin, 16 [&] (1994). 5. A. R. Brugh and A. Atkinsn, Sdium Silicate Based. Alkali-activated Slag Mrtars: Part I. Strength, Hydratin and Micrstructure, Cem. Cncr. Res., (00). 6. K. J. Mun, Prperties f Nn-sintered Cement and Cncrete Recycled with Industrial Waste(in Krean), pp. 0 in Ph. D. Thesis, Chnbuk Natinal University, Krea, S. H. Lee and Y. B. Mun, Prperties f Reactin Rim n Blast Furnace Slag Grain with Alkali Activatr Accrding t Hydratin Reactin(in Krean), J. Kr. Inst. Resurces Recycling, 18 [] 4-8 (009). 8. G. J. Kim, H. G. Han, D. S. Se, and J. K. Lee, Shell Pwder Cating n the Surface f Cncrete by Geplymer Cement(in Krean), J. Kr. Mater. Res., 0 [1] 1-6 (010). 9. P. C. Hiemenz, Principles f Cllid and Surface Chemistry, J. Cllid and Interface Science, 70 [] (1979). 10. C. Y. Lee and S. Y. Bae, A Study fr the Use and Accelerating Demand f Fly ash (in Krean), J. Kr. Cncr. Inst., 8 [1] 50-5 (1996). 11. F. M. Lea, The Chemistry f Cement and Cncrete, pp , Chemical Publishing Cmpany, Inc., New Yrk, w wz

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