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    CEMENTano CONCRETE RESEARCH Pergamon ‘Cement and Concrete Research 291999) 1611-1617 Formation and hydration of CS prepared by microwave and conventional sintering Haoxuan Li, Dinesh K. Agrawal, Jiping Cheng, Michael R. Silsbee* Merial Researok Laboraiort, The Penussvania State Unversity, Unversity Park PA 16802, USA Received 9 October 1998: cepted 15 Jone 1999 Abstract, A microwave sintering method was used to prepare C\S from precipitated CaCO, Ludox (SiO), and AKOH)s ot Fe,0,. Brunauer- Emmett-Teller (BET), X-ray diffraction, scanning electron microscopy, and calorimetry were used to characterize the sintered samples, ‘The results indicate that heating rate played a very important role in C,$ formation in conventional sintering. Microwave sintering re- salted in improved formation of C,S compared to conventional sintering, even atthe same heating rates, After sintering at 1500°C sam ples prepared using microwaves were still porous, with a specie surface ares of about 0.4 m/g, Microwave formation of C:S was achieved At temperatures as low as 1350°C when using ALLO, additions. The use of Fe,O, at an additive was not as effective in promoting C.S for- ‘mation as expected. Microwave effects on sintering as well as the sintering setup are also discussed in this paper. © 1999 Elsevier Sci- ence Lid, Al rights reserved. “Keywords Microwave orering: Ticaeum sh 1. Introduction In 1983, Quéméneur, etal. reported the feasibility of us- ing microwaves to process Portland cement clinker [1]. In recent years others have reported the use of microwave clink= ering [2-4] to form a variety of cements, In the Portland co- ‘ment clinker system there are many components that are helpful to CS formation because the melt phase occurs at high temperature, promoting ion diffusion. The microwave ‘energy absorptions [5] of the pure oxides of the elements that make up Portland cement clinker have been character ized. However, the behavior of complex systems such as those found in cement clinkering especially involving solid- state reactions is less well characterized. Conventional prep aration of C:S requires a high sintering temperature and long holding time [6] due to the low ion diffusion rates for solid-state reactions. The goal of the study described here was to lower the required sintering temperature and to re- duce the holding time. Typically using a multimode microwave cavity for sin- tering causes problems with unstable temperature measure- ‘ment due to energy discharges, as well as the nonuniformity in sinteting due to localized heating. In our work, we have attempted to make some improvements in these areas, * Corresponding ashor Tels (814) 865-0285 fox: (814) 863-2326, E-mail addres: slsee pac (M. Silsbee) Conventional cement notion i eed throughout. \e:X-rydifection: Calorimetry 2. Methods 2.1. Starting materials Precipitated CaCO, and colloidal SiO: (Ludox, SiO, 40%) were used for C,S production. ANOH), and Fesoy were used in small amounts. On an as-sintered basis the ad- ditives were used as follows: No. 1 series: ALO; = 0.85% No. 2 series: AlOs = 0.5, 1.0, 15, and 2.0% No. 3 series: Fe;0; = 0.5, 1.0, 15, and 2.0% 2.2. Sample preparation The starting materials were put into a plastic beaker and hhand-mixed for about 20 min. The doughy mixture then was Put into a foil container, vibrated, and then dried at 105°C for ‘th. The dried “cake” was cut into the desired dimensions. 2,3. Microwave and conventional sintering setup ‘The microwave sintering setup has been described else- where [2]. A high heating rate electrical furnace was used (0 obtain average heating rates of 41 to S6°C/min. A general purpose electrical furnace was also used for conventional sintering at an average heating rate of ~8°C/min. A type S thermocouple wrapped with platinum foil and well grounded was used to monitor the temperature in the microwave chamber. The holding time at maximum temperature was 10 ‘min for all samples. ‘00-§816/99/5 se font mater © 1999 Elever Science Lid Al ight eseve. ‘Pll, S0008-8846(99)00 145-3 ten 1H. Lier ak / Cement and Concrete Research 291999) 1611817 W158 “20 353035404550 Heating time (minutes) Fig. Temperate curve in discharge. 3. Results and discussion 3.1. Microwave sintering process improvements Discharge is often encountered when sintering in a multi- ‘mode cavity. The effect of the discharge phenomenon on Temperature measurement when using a thermocouple is il lustrated in Fig. 1, which shows that the discharge causes the thermocouple readout to fluctuate. When discharge is severe, it causes damage (o the sintering packet and thermo- couple. In order to overcome this problem the following steps must be taken: |. Optimize the mass of the sample (7) 2. Expose the sample directly 1o the microwave field (no crucible). 3. Carefully align the sintering packet (and sample) along the vertical atis of the microwave cavity. 4, Ground the thermocouple. 5. Optimize the heating rate. 1600 3 Specific surface area (m’/g) 1600 & 1 , “ 900 1000 1400 1200 1300 1400 Sintering temperature (°C ) 0 Fig. 3.No. {series siface area developmen: with sinringemperause. With the above measures the discharge was eliminated, as shown by the improved sintering temperature curve in Fig. 2, 3.2, Sintered surface area development ‘A MonoSorb Surface Area Analyzer (model MS-12, a Product of Quantachrome, Boynton Beach, FL, USA) was used for Brunaver-Emmett-Teller (BET) surface area mea- surements, Fig. 3 shows the surface area development in the first se= rics (0.854% Al,05 addition). The change in BET surface ‘area was apparently linear with increasing temperature up 10 1350°C. In the system C,S-C:S-C.A, the lowest temperature at which a liquid can be expected to form is 1455°C, When the liquid forms, the surface area should decrease quickly. ‘There was no noticeable change due to the formation of liq- uid observed in our samples, suggesting that the changes o°- curring were due to solid-state reactions. The samples were a 2 Fe, addition | So E asi © 1200 & 0 Bt Eso) | «gis a E 5 Boor 2, = 400} 2 1,0, addition a Bos 0 ee 0 5 10 13 20 25 40 38 40 45 50 Ibeaers Os-reeLe Nene Larner -ecL as Heating time (minutes) Fig. 2 Smproved tempersue curve, Additive addition percentage Fig 4 No.2 and 3 saris surface area development with adv addition Leta. Cement and ConereteRescarch 2941999) 1611-1617, 1613 2.0% Al,O, 05% ALO, 6 50 35 Fig. 5. Conventional, 100°C (Cima) (3) C5. (2) BetwC3S, (1) C20, found to be porous even when sintered in microwave at 1500°C. The surface area was much higher (about 0.4 w/z) than that of commercial clinker Fig. 4 shows the surface area development of No, 2 and 3 series of samples that were microwave sintered at 1350°C, ‘AS the content of Al,O, was increased, the surface area de- creased while the FeO; addition had an opposite effec, 3.3. Phase composition {A Scintag PAD V diffractometer (Cupertino, CA, USA) in conjunetion with a computerized calculation program was used for X-ray diffraction (XRD) phase characteriza tion. Cu Ka. A = 1.54059 A and a scanning ite of 228) 25 35 ‘min were applied. Sample size was controlled at 0.25 g to ‘minimize sample-to-sample variations, 3.3.1. Conventional sintering Fig. 5 shows the XRD patterns of No. 2 series of samples sintered with an average heating rate of 8°Cimin, In this set of samples, only B-C.S and CaO were detected, In the C,S- C:S-CsA system the liquid phase appears only ata tempera tures of 1455°C or higher, making it dificult to form CyS at lower temperatures. Fig. 6 and Fig. 7 show the XRD patterns of No. 2 series samples sintered conventionally at higher heating rates. In both situations CS formed. It should be noted that the heat- ing rate was even more important than the final sintering 45 50 55 Fig 6. Conventional, 450°C (41°CInin). 8) CS, 2) beawS, (1) C20. vos HU eral /Cement and Conerete Research 29( 1999) 1611-1617 25 30 35 2.0% ALO, 2 Fig, 7 Conventional, 400°C (S6°Cimin). BHC, (2) bei-C.8, (1) C20, a) gure, temperature since the CaO content (intensity) was less at ‘56°C per minute (Fig. 7) than at 41°C pee minute (Fig, 6). ‘But with higher heating rate and lower additive addition (AlO, = 0.50%), the sample had a higher surface area and B-C,S changed to ’—C;S as shown in Fig, 7 (bottom curve). 53.3.2. Microwave sintering Figs. 8,9, and 10 show the XRD patterns of No, 2 series of samples; when sintered at 1300°C the samples contained C,S. As the sintering temperature was raised, the CaO content was reduced, and C,$ content increased. But the dramatic 25 30 35 LM development occurred at 1350°C. It should be noted that even at 1300°C the microwave-sintered samples contained less CaO compared with samples conventionally sintered at 1400°C or higher, showing the advantage of microwave sin- tering. The other characteristic was thatthe identical peak of CyS (d = 3.04 A) was widened, indicating C38 amorphous structure. Its morphological observation by scanning elee- tron microscopy is shown ia Fig. 11 ‘The XRD patterns of No. 3 series of samples (containing Fe,0,) are shown in Fig. 12. The CaO content in these sam: piles was higher than that with ALO, addition excepe for the 2.0% Fe,0; addition, 15% ALO, 45 50 55 Fig. 8 Microwave, 300°C: (3), (2) beta C.S, (1) C0, 1H. Li etal Cement and Concrete Research 29(1999) 1611-1617 tos 2.0% Al,0, “| 15% A1,0, 1.0% ALO, a 50 55 Fig. 9. Microwave, 390°C. 6) 35, 2) bet.C38, (1) C40), 34. Calorimetry A Thermonetics SEC calorimeter (model SEC ¢12-45- 2E, witha refrigerated bath and circulator) was used for eal- ‘orimetry experiments. All samples for calorimetry were passed through a No. 325 sieve and used a water/eement ra- 1.00, The hydration temperature was 25°C, Fig. 13 shows hydration heat evolution of C,S conven- tionally and microwave sintered at 1400°C or higher, It is, obvious that microwave-sintered C,S showed a shorter in- duction period in early hydration while maintaining the same total heat evolution. This demonstrated that micro- wave-prepared C\S containing Al,O, had higher hydraulic reactivity. On the other hand, microwave-prepared C,S con- taining Fe,O, showed a rather long induetion period and. Jess heat evolution during early hydration, as shown in Fig. 14, indicating the restriction of early hydration by the Fe,O, additive 4. Diseussion From conventional sintering results it has been shown that heating rate played a very important role in solid-state CS formation. With a low heating rate (8°C/min, which js common in many laboratories throughout the world) CS is difficult to form in solid-state reaction. As the beating rate is increased, raw mix components’ decomposition or phase transformation overlapped with product formation, which may be called “thermal activation”: the newly formed, im- 1.0% AO, 0.5% ALO, | 50 35 Fig. 10. Microwave, 14°C. (3) CS, 2) bew-CS, (1) 20. vo16 H.Li etal. / Cement end Concrete Research 291999) 1511-1617 Fig 11. Misowve, 1INFC: ALO, = 20% perfect structure reactants take part in reaction quickly, leading to casy occurrence of solid-state reaction I is clear that the microwave generates rapid sintering. Besides this, a microwave processing has still other advat tages, which greatly facilitate C\S formation in solid-state reaction, The following are some of the features. 4.1. Volumetric (bulk) heating tional sintering, The sample can be sintered more uniformly in.a microwave field. 4.2, Selective heating Microwave heating efficiency is closely related with the relative dielectric constant (¢,) and loss tangent tan 8) of the sample. The absorbed power can be expressed in the fl owing Eq. (1) of Ea. 2) (7h Microwave can penetrate into the sample and beat is en- Tee eraed throughout the whole sample. Therefore microwave” ~ 28/€9¢,'tan 6 [Et a sintering is less dependent on heat transfer than is conven- Pee,’ tan 3 @ 2 32 2 2.0% Fe,0, pas 2 | KA 7 SHHet 1.5% FeO, \ 1.0% Fe,0, Me 05% Fe,0, 22 0.0% Fe,0, 30 55 Fig, 12. Microwave, 50°C. 3) CS. 2) bets-C3S. (1) C20. mV/gram sts as Hydration time (hours) Fig. {3 Myon tevin of supe sea AMM and 380 tanx¥or tan 8 will absorty vane Inierowave energy. As the temperature rises, €/° and tan ‘ca also become grees, eventually resalting in a phenome toon known as “thermal runaway. Ini cement raw mix system crystalline SiO. (quart?) is the not themlly inert component I has been reported that SiO, was loys micrenvave-cnergy’ recxplive uf Jower temperatare [5] tind the tan 8 of SiO, increased yeeatly ay the temperature rises above |10U°C [71 I has aso been reported that SiO, Isl Components with greater e gels heat ana welt qvickly during microwave sinterin ok Bleenie field effect In solicestate reaction one of the most important fyetors affecting veut tering jon diffusion is tess important due tothe Tack oli til phase. Mierowaves are a high-frequency electric tied with which ions interact, lealing to the inerease of fon Ui sion and improving solid-state rexetion te is ion diffusion, In conventional sit In auktion, as it bus been shown, avierowave-prepareit ©,8 with ALO, ublition bad 9 shorter induetion period dur ing early hydration, that is, the acceleration period ot CS hnydrwion aceurted garter than the conventionally sintered cones. Ie gas reported! that ALLO, alitions in CS ted 0 higher hydraulic reactivity [9]. Therefare, the possible im plication is that in microwave ek ALO, is more active sand ore of the ALLO, is included in the C,S structure, pr ducing a more aetive alte as a sintered produ 5. Conclusion 1. Heating inn ad very i portant role in solid-state formation ot C\S. With low heating rates C8 was difficult form even a HOO" ance OF a Hqulid phase, 2. Mierowave-sintered C,8 containing ALO, hub been Formed at temperatures slow as 1300°C, and was the i by 1350°C. Ady Do LO%ALO, aesatp, | Lame, 20S Bu eeEle! Hydration time (hours) ig Haddon ten of umples nse nore BS \wave sintering promoted much of the C$ formation via solid-state action. 3. Micrwave-prepared CS containing ALLO, showed i perival daring early hydration, whieh 1s ancoxporation of ALO, unto the CS shorter inductio nay be de 6 steucture 4. The etieet of Fe,0, on CS formation was not as Ft vorable as expected; C,S eomtaining FeO, bad longer inuluction periods and lower beat evolution during cealy hy ration, Acknowledgments “This research was partly supported by 2 sesearch grant 1 the Elecisie Power Research Institute, whicl is 2 y acknowl négew, J. Che, Rave, Mision ans ake ih pple, As Cr Sue 612) 298 BSS, Yh A Soa, DM Ky, Mame sins tI lta Lets 27 149969 135-159 IHL, Fame DM Ros, K. oy, Sletowive clkering of vinary

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