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1 Jurnal f the Krean Ceramic Sciety Vl 46, N 3, pp 75~81, 009 DOI:104191/KCERS Prus Materials frm Waste Bttle Glasses by Hydrthermal Treatment Dng-kyu Lim and Eun-Tae Kang Schl f Nan & Advanced Material Science and Engineering, Engineering Research Institute Gyengsang Natinal University, Jinju , Krea (Received January 8, 009; Accepted February 6, 009) w s œ y ³Á k w ù Á œw, œw ( ; ) ABSTRACT Prus materials were manufactured by hydrthermal treatment f waste bttle glass withut fam agent Factrial design was applied t analyze data by statistical methds and deal with the imprtant factrs fr a prcess The largest effect fr prsity was fr temperature f hydrthermal treatment Amunt f water and temperature-water interactin appeared t have little effect The particle size f raw material was als identified as a majr factr by ne-way ANOVA and the prsity decreased as the size increased The sintering temperature was nt statistically significant fr the prsity but was significant fr the pre size The prus material had cmpressive strength and thermal cnductivity cmparing with thse f ALC (autclaved lightweight cncrete), althugh it has higher prsity than fr ALC Key wrds : Waste bttle glass, Prus materials, Hydrthermal treatment, Factrial design, Prsity 1 s» w w m ƒ š w» s» y»» w š w œ x w 1) w s y % y % ƒ 003 y 903% e w s y s, m qp yw w glass qp, m yww glass, glass, glassk, glass bead, s w s y w» w y, Glass-ceramicy, w y œ 1000æ š w { w y»w» q y w s CaCO 3, dlmite (CaCO 3 MgCO 3 ), SiC, š»š s ùy CO ƒ w Crrespnding authr : Eun-Tae Kang Tel : Fax : Sigli ) 450 C x ü»œ x w ù œ w 00 C autclave y w g s w ƒ r w yw j w e š 3) ü w k w Ÿ ww Schlze 4) ³ 3 OH w µm, µm 45 µm ƒƒ free OH grup, w w OH, š w w OH w vj šw Ernsberger 5) w 9 µm vj š w w Tmzawa 6) w w w H O/OH ƒ j š šw»œ w» w { v w, w w OH w w w x z mw ƒ,, š n s j»»œ 75

2 76 ³Á k w e w»œ m mw» œ š ³ w œ wš w x s w œ œ»œ w e w,, š n s j» wš, 3ƒ xw x z ƒ x w w j» e w e mw w w s j» w ƒƒ e mw w 1 w» w 3 e z œ» œ w w š 3 10 wt%, 15 wt%, 0 wt%, 160 C, 00 C, 40 C wš 3z w, ù n s j» 106 µm w 750 C š w œ»œ w w»œ d w 3 w r j d w w x» w y w ww n s j» w w z n j» w» w j» 45 µm w, 45~75 µm, š 75~106 µm 3 w x, 750 C š w w e ww n j» w w 3 w s w œ w» w n s j» š w z 690 C, 70 C, 750 C, 780 C 4 w œ w w»œ»œ j» w w e w,»œ j» Mercury Prsimetry(Aut Pre 9500, Micrmeritics) d w Fig 1 FT-IR spectra f parent waste bttle glass and glasses hydrthermally treated at varius temperatures 4 s w œ œ r œ s w s 300 g 3 w sieve(45 µm, 75 µm, 106 µm) w ƒ w autclave w 6 w z w s w 106 µm sieve mw ƒ w 750 C 30 w œ w 5 Ÿ» (VERTEX 80 v, Bruker) š û s ƒ» w w w s s KBr pellet w 4000 c -1 ~400 c -1 4c w -1 d w, k s» we {»s w š y ù r» w TG DTA 5 C/min ƒ 1000 C¾ d w XRD (D/max-3C, Rigaku) w œ» w œ 45 µm w w X z w, SEM (JSM-6400, JEOL) œ t w Lee s disk w 7) d w 3 š 31 s w s autclave w we k w» w s wì Ÿ» w wz

3 w s œ y 77 Fig DTA and TG curves f hydrthermally treated glass d w Fig 1 ùkü w 3600 cm -1 (8 µm), 350 cm -1 (43 µm), š 1645 cm -1 (61 µm) vj j y š cm vj û q ¾ r s j š vj cm Si-OH(free OH) w 4,8) 3300~3500 cm -1 O-H 5,8,9) cm sw wš š z ³ w w cm m , 360, 1870 cm vj ùkü š 10) ù Uchin 9) autclave y cm O-H w š w z Fig cm vjƒ Uchin vjƒ w -1 vj w w k w š q w 1645 cm H-O-H w š l 5,8,9) s ü we y w w Fig 1 ƒ ƒw cm s q w š cm š l ƒ ƒw SiOH ƒw Fig 00 C s TG DTA 10 C w w w 30 C w w w 300 C 400 C w w ùküš Uchin 9) w w ³ k k w IR w w 00 C k ƒ ú Fig 3 XRD pattern f prus materials manufactured by hydrthermal treatment ( cm ) -1 (1645 cm ) -1 ƒ wš, -1 00~400 C 3600, 800, 350, 1670 cm ƒ w š šw w 10 C w w Fig 1 w w vj cm 1645 cm k, 30 C 350 C w w w w O-H k w q š 300 C 400 C w s w» ky w ƒ w 730 C yƒ û ùkü w 750 cm 30 w»œy ww w Glass-ceramic yw p w, w Fig 3»œ XRD vj y w, w yƒ Wllastnite(CaSiO 3 ), devitrite(na Ca 3 Si 6 O 16 ), š quartz, Na O-CaO-SiO k 11) ew 3 ƒ m w» w ƒ x»œ w w»œ ƒ r l d s³ w Table 1 Minitab m v w w ùkü ( ) ( ) š ( ) P 005 w m w, 9997% R» R z w ùk 46«3y(009)

4 임동규 강은태 78 Analysis f Variance fr Prsity with Temperature and Distilled Water Surce DF Sep SS Adj SS Adj MS F Temp Water Temp Water Errr Ttal S = R = 9997% R = 9995% DF : Degrees f freedm, SS : Sum f squares, MS : Mean squares, F : Test statistic, P : p-value, S = MSE (errr mean f squares) R : predicted R, R : adjusted R Table 1 P p a p a 열반응온도의 조합에 대한 평균 기공율을 이들 인자에 대 해 나타낸 그림이다 이 그림으로부터 수열반응온도는 기 공률에 매우 중요한 인자인 반면 증류수량은 거의 영향 을 미치지 못함을 명확하게 알 수 있었다 기공률에 대한 온도 증류수 의 상관효과도 기공률에 영향을 미치지 못 하는 증류수량 때문에 상호작용이 크지 못한 결과를 나 타내었다 는 수열반응 온도와 증류수 첨가량을 달리한 수 열처리로 생성한 기공재료의 표면미세구조로 는각 각 증류수량 첨가하여 온 도에서 수열 반응시킨 폐유리로 만든 다공질 재료의 표 면 미세구조이며 는 각각 증류수량 온도에서 수열 반응시킨 첨가하여 폐유리로 만든 다공질 재료의 표면 미세구조이다 같은 온도에서 증류수량의 증가에 따른 기공의 크기에는 큰 변 화가 없었으나 골격 내에 작은 기공들이 생성되는 것을 볼 수 있었다 이 작은 기공의 생성은 에서 더 많이 생성되었다 이는 앞의 적외선 분광분석 결과에서 보이듯 보다 에서 결합이 더 많은 것을 고려하 고 등 의 결과를 인용하면 수열반응 시 강하게, ( ) Fig 5 a, b, c 10 wt%, 15 wt%, 0 wt% Fig 4 Variatin f prsity with temperature and amunt f distilled water 내는 값으로 의 R 은 기공률에 대한 데이터의 변 동중 가 회귀 모델로 설명 될 수 있음을 의미한 다 이를 통해 수열반응에 증류수와 반응온도 및 이들 인 자의 교호작용이 통계적으로 유의한 영향을 미침을 알 수 있었다 는 분산분석표로는 명확하지 않은 각 인자 들의 효과 정도를 분명하게 보여주기 위해 증류수량과 수, 9997% 9997% Fig 4 Fig 5 d, e, 00 C f 10 wt%, 40 C 15 wt%, 0 wt% 40 C 00 C 40 C Uchine SiOH 9), Surface micrstructures by SEM f prus materials sintered at 750 C with hydrthermal treatment: (a) 00 C 10 wt% distilled water, (b) 00 C 15 wt% distilled water (c) 00 C 0 wt% distilled water, (d) 40 C 10 wt% distilled water, (e) 40 C 15 wt% distilled water, and (f) 40 C 0 wt% distilled water 한국세라믹학회지

5 w s œ y 79 Fig 6 Appearance f prus materials with particle size Fig 8 Variatin f prsity with particle size fr prus material Table Analysis f Variance fr Prsity with Particle Size Fig 7 Variatin f bulk density with particle size fr prus material w OH» w w 00 C»œj»ƒ 40 C j 40 C 00 C ƒ w k ü w w, Ÿ ew l 00 C 0 wt%»œ w 33 j» w n j» w» w j» 45 µm w, 45~75 µm, 75~106 µm 3 ù š 750 C š w w œ Fig 6 ùkü sizeƒ ƒ w sƒ ù y w Fig 7 8 j w r d s³»œ v j» w ùkü j»ƒ ƒ w v ƒwš»œ w Fig 6 ew j»ƒ j t»s k Surce DF SS MS F P Particle size Errr Ttal S = 618 R p = 947% R a = 937% SS : Sum f squares, MS : Mean squares,» Table»œ n j» w w e P 005 w 0000 j» w m w w R 947%»œ w l 947%ƒ z ùkü ƒ»œ ƒw 34 w 45 µm w j», 00 C 0 wt% š wš œ 690 C, 70 C, 750 C, 780 C, 810 C 5 w œ w r»œ w e, P 005 w 00 w ƒ ù z w ùkü R 3744% û, z»œ w w w š w s³»œ j» Fig 9 ƒ ƒ w»œ j»ƒ f 46«3y(009)

6 80 ³Á k Fig 9 Variatin f average pre diameter with sintering temperature fr prus material Fig 10 Cmpressive strength versus sintering temperature fr prus material ƒ»œ w ƒ w ù» ƒ e w 0000 P, 919% R l s³»œj» w w m w w œ»œj» w œ Fig 10 ùkü 690 C ƒ 7471±111 kgf/cm ƒ ƒ w û»œ yƒ œ ü s³»œ j»ƒ ƒw w»œ j»ƒ ƒw û»œj» Fig 11 Thermal cnductivity versus sintering temperature fr prus materials w œ hydrxyapatite ùkù š 1) Fig 11 œ y ƒ ƒw w 780 C ƒ û 0031±0003 kcal/hm C ùkü»œ ƒw w š ù, 13) r»œ m w e w ƒ ƒw»œ j» y w ƒ š 4 s CO ƒ j s mw œ w x z y w m j»ƒ»œ ƒ w, w e w yƒ û,»œ w e wù»œ j» w e œ œ»sgj p v w ùkü REFERENCES 1 Krea Glass Industry Cperative, F A Sigli, F Felician, M V Gitt, M R Davls, and M J Junir, Prus Silica Matrix Obtained frm Pyrex Glass by Hydrthermal Treatment: Characterizatin and Nature f the Prsity, J Am Ceram Sc, 86 [7] (003) 3 E N Buls and N J Kreidl, Water in Glass : A Reiew, w wz

7 w s œ y 81 J Can Ceram Sc, (1970) 4 H Schlze, Incrpratin f Water in Glasses : I, Glastech Ber, (1959) 5 F M Ernsberger, Mlecular Water in Glass, Am Ceram Sc, 60 [1-] 91- (1977) 6 M Tmzawa, Water in Glass, J Nn-Cryst Slids, (1985) 7 R F Pwell, A Realistic Apprach t Labratry Thermal Cnductivity Experiments with Slids, Phys Educ, (1969) 8 R F Barthlmew, B L Butler, H L Hver, and C K Wu, Infrared Spectra f a Water-Cntaining Glass, J Am Ceram Sc, 63 [9-10] (1980) 9 T Uchin, T Sakka, and M Iwasaki, Interpretatin f Hydrated States f Sdium Silicate Glasses by Infrared and Raman Analysis, J Am Ceram Sc, 74 [] (1991) 10 D P Zaburin, Infrared Spectra f Hydrgen Bnded Hydrxyl Grups in Silicate Glasses A Re-interpretatin, Phys Chem Glasses, 40 [4] (1999) 11 G W Mrey and N L Bwen, High SiO Crner f System Na O-CaO-SiO, J Sc Glass Technl, (195) 1 D M Liu, Influence f Prsity and Pre Size n the Cmpressive Strength f Prus Hydrxyapatite Ceramic, Ceramics Internatinal, 3 [] (1997) 13 G Buntebarth and J R Schpper, Experimental and Theretical Investigatins n the Influence f Fluids, Slids and Interactins Between them n Thermal Prperties f Prus Rcks, Phys Chem Earth, (1997) 46«3y(009)

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