Effect of Calcium Addition at High Temperature on

Fly Ash’s Activation Character

LUO Zhongtao1,aˈZHANG Lei2,b, YANG Jiujun3, bˈWANG Kai4, c, d
a
School of Materials Science and Engineering, Zhengzhou University, Zhengzhou 450052, China. luozhongtao@126.com
b
Department of Materials Engineering, Tianjin Institute of Urban Construction, Tianjin 30038, China. yangjjun@zzu.edu.cn
c
Shool of civil Engineering and Architecture, East China Jiaotong University, Nanchang 330013, China. wklab@163.com
d
School of Materials Science and Engineering,, Southwest University of Science and Technology, Mianyang 621010, China

Abstract—The surface network structure of fly ash modified by ೒ 1 Ў CaO-SiO2-Al2O3 ϝ‫Ⳍܗ‬೒ঞ৘⾡⸙䪱䋼㛊‫ޱ‬ᴤ

calcium addition at high-temperature was analyzed by NMR, and ᭭೼ϝ‫Ⳍܗ‬೒Ёⱘऎඳ㣗ೈDŽ⬅೒ৃⶹˈ৘㛊‫ޱ‬ᴤ᭭ⱘ∈
Ka method-㧔ICP-AES㧕 rapid evaluation was used too. By ࣪⌏ᗻѺे㞾䑿∈⹀ᗻϢ݊ CaO ৿䞣ᄬ೼Ⳉ᥹݇㘨DŽF 㑻
activity exhibition of modified fly ash in cement paste, the effect ㉝✸♄Ёⱘ CaO 㒱໻䚼ߚᰃ㒧ড়Ϣ⦏⩗ⳌϢ᱊ԧⳌЁˈ
of calcium addition course at high-temperature on fly ash’s Ca2+ᰃϔ⾡㔥㒰㒧ᵘ᷵ℷ⾏ᄤˈৃҹᬍব㉝✸♄⦏⩗Ⳍⱘ
activity characteristics was studied. The results indicate: 㒧ᵘঞ SiǃAl ⱘ䜡ԡ⢊ᗕՓ⦏⩗Ⳍ㒧ᵘ᮴ᑣ࣪๲ࡴˈᦤ催
modified by calcium addition at high-temperature, fly ash’s early
⦏⩗Ⳍⱘ⌏ᗻDŽৠᯊˈCa2+೼ϔᅮ⦃๗⢊ᗕϟৃҹᠧᓔ Si-
Ka value improvement, and ratio of activated Al2O3/SiO2 was OǃAl-O 䬂ˈᦤ催ᭈϾԧ㋏ⱘ࣪ᄺ⌏ᗻ[2,3]DŽᴀ᭛Џ㽕䗮䖛
more than twice the average ratio of original fly ash, indicating 催⏽๲䩭䖛⿟ᇍ㉝✸♄䖯㸠࣪ᄺ⌏ᗻ▔থˈᑊ‫ ࡽ׳‬K a ⊩
the calcium addition course at high-temperature was not only
destructive on Si-O bond, its destructive power on Al-O bond was ⦃๗ঞ∈⊹‫⦃⌚ޔ‬๗ⷨお݊ᬍᗻৢⱘ⌏ᗻ⡍ᕕDŽ
also more apparent. Under the environment of cement paste,
modified fly ash’s reaction took place rapidly at early stage of II. ᅲ偠ॳᴤ᭭Ϣᮍ⊩
cement hydration, and continually to consume Ca(OH)2
produced by cement hydration.
A. ॳᴤ᭭
Keywords-fly ash; calcium addition; depolymerization; activity 䞛⫼ⱘ∈⊹ᰃ℺∝Ѯϰ∈⊹᳝䰤݀ৌ⫳ѻⱘ P.O 42.5
characteristics 㑻᱂䗮⸙䝌Ⲥ∈⊹˄ OPC˅ˈ݊ 95%ⱘ乫㉦㉦ ᕘᇣѢ
43.50ȝm˗㉝✸♄䗝⫼℺∝䰇䘏⬉ॖѻⱘ᱂䗮Ԣ䩭㉝✸♄
I. ࠡ㿔 ( ㅔ ⿄ LCFA) ˈ ᳔ ৃ ޴ ㉦ ᕘ 40ȝm ˈ ↨ 㸼 䴶 ⿃ Ў 370
ࠡᳳⷨお[1]Ёˈ䗮䖛㉝✸♄乫㉦೼ K a ⊩⦃๗ϟⱘ m2/kgˈ䳔∈䞣↨Ў 108%ˈሲѢĊ㑻㉝✸♄ˈ݊࣪ᄺ㒘៤
㾕㸼 1DŽЏ㽕䞛⫼࣪ᄺ㒃 CaOˈ৿䞣ϡᇥѢ 99.5%DŽ
SEM ᔶ䉠ব࣪ৃⶹ⒊㱔⌏࣪⚍ᰃ㉝✸♄乫㉦㸼䴶 Si-O-Al
㔥㒰㘮ড়ԧ㸼㾖⌏࣪㛑㭘ᔅऎඳˈৠㄝডᑨᴵӊϟˈডᑨ Table1 Chemical composition of fly ash
೼⌏࣪⚍໘᳔‫ܜ‬䖯㸠ˈ䖯㗠৥਼䖍ᠽሩDŽᭈϾ䖛⿟Ё⒊㱔 ࣪ᄺ㒘៤ wt/ˁ
ॳᴤ᭭
SiO2 Al2O3 Fe2O3 CaO MgO SO3 R2O IL
⌏࣪⚍ߎ⦄ৢ߭࣪ᄺ⌏ᗻডᑨ䖯⿟ᯢᰒ๲ᖿDŽ಴ℸ䞛প᳝
OPC 21.04 6.94 2.36 61.27 2.64 1.94 0.83 3.76
ᬜ᥾ᮑᇍ㉝✸♄ⱘ㸼䴶㔥㒰㒧ᵘ䖯㸠ᬍᗻˈ䰡Ԣ݊㘮ড় 50.80 28.51 7.06 3.94 1.10 1.68 2.96 2.65
LCFA1
ᑺǃ㸼㾖⌏࣪㛑ৃҹ๲ࡴডᑨᴵӊϟ⒊㱔⌏࣪⚍ⱘߎ⦄޴
⥛ˈҢ㗠ᦤ催㉝✸♄ㄝ⸙䪱䋼㛊‫ޱ‬ᴤ᭭ⱘডᑨ⌏ᗻDŽ B. ᅲ偠ᮍ⊩
催⏽๲䩭㒣ࠡᳳⷨおӬ࣪ৢЎ‫݋‬ԧ䜡↨Ў
81.0%LCFA1+15.0%CaO+3.0%⷇㝣+1.0%㧸⷇ˈ⏽ᑺࠊᑺ
Ў 1200 ćϟ 0.5 ᇣᯊDŽᑊ‫ࡽ׳‬फҀᎹϮ໻ᄺⱘ AV400D Ḍ
⺕݅ᤃ䈅˄NMR˅Ҿ䖯㸠㉝✸♄㸼䴶㔥㒰㒧ᵘ㾷㘮ߚᵤDŽ

⌏ᗻ⡍ᕕߚᵤЏ㽕⍝ঞ K a ⊩⦃๗ঞ∈⊹‫⦃⌚ޔ‬๗DŽ
⊩⦃๗ঞ݊䅵ㅫ‫݋‬ԧখ✻ࠡᳳⷨお[1,4]ˈᑊ䖯㸠ᠿᦣ⬉ᄤ
ᰒ ᖂ 䬰 ˄ SEM ˅ ߚ ᵤ DŽ ᦎ ㉝ ✸ ♄ ∈ ⊹ ‫ ⦃ ⌚ ޔ‬๗ 䆒 䅵
(FA/CFA3-2)䞛⫼ 0.40 ∈♄↨ǃ㉝✸♄ᦎ䞣↨՟Ў 45%DŽ
៤ൟ䆩ӊሎᇌЎ 40mm×40mm×40mm ゟᮍԧˈ䆩ӊ៤ൟ
1d ৢᢚ῵ˈ㕂Ѣ‵㛊༫Ёᆚᇕ˄䱨㒱∈ߚ˅‫ݏ‬ᡸˈࠄ㾘ᅮ
Fig.1 Activation distribution of materials in CaO-SiO2-Al2O3 system

978-1-4577-0290-7/11/$26.00 ©2011 IEEE

5896
啘ᳳপߎ䖯㸠ᡫय़ᔎᑺ⌟䆩ˈᑊপḋ䖯㸠㉝✸♄ডᑨᑺ⌟ B. K a ⊩⌏ᗻ䆘Ӌ
ᅮ˄GB/T 12960-1996˅ǃX ᇘ㒓㸡ᇘ˄XRD˅ߚᵤDŽ
100 100
III. 㒧ᵰϢߚᵤ LCFA1 Ka

29
CFA-4 Ka
A. Si/27Al NMR ߚᵤ
80 LCFA1 Al/Si 80
೒ 2 ੠೒ 3 㒣催⏽๲䩭ৢ㉝✸♄ⱘ 29Si/27Al NMR 䈅DŽ

⌏ ᗻ A l2O 3/S iO 2
CFA-4 Al/Si
⬅೒ 2 ৃ㾕ˈLCFA1 ⱘ⸙⇻ಯ䴶ԧᄬ೼ Q1ǃQ2ǃQ3 ঞ Q4

K aؐ /%
޴⾡㘮ড়ᗕˈ݊Ё Q3 Ϣ Q4 ⱘዄؐ䕗ᆑϨᯢᰒˈ䇈ᯢॳ⢊
60 60
㉝✸♄ⱘ⸙⇻ಯ䴶ԧ㘮ড়ᑺ䕗催DŽCFA-4-1200ćⱘ෎ᴀ䲚
ЁЎ Q1 ⱘ⡍ᕕዄˈϨዄᔶবじѺ๲ᔎˈ⸙⇻ಯ䴶ԧ㘮ড়
ᑺᯢᰒ䰡ԢDŽ⬅೒ 3 ৃ㾕ˈॳ⢊㉝✸♄ⱘ䪱⇻໮䴶ԧ㒧ᵘ
40 40
ҹ 6 䜡ԡ˄࣪ᄺԡ⿏ į 㑺Ў-20 ppm˅੠ 4 䜡ԡ˄࣪ᄺԡ⿏
į 㑺Ў 30~40 ppm˅ᮍᓣᄬ೼DŽ㗠 CFA-4-1200ć೼࣪ᄺԡ
⿏ į-20 ppm 䰘䖥ⱘዄؐ෎ᴀ⍜༅ˈ㗠೼࣪ᄺԡ⿏ į30~40
20 20
ppm ໘ⱘዄؐᯢᰒࡴᔎ [5] DŽ䖯ϔℹॄ䆕ⳌᇍѢॳ⢊㉝✸
♄ˈ㒣䖛催⏽๲䩭ᬍᗻৢⱘ㉝✸♄݊ᔎዄ㒓ԡ⿏ᳱℷؐᮍ 1d 3d 7d 14d
৥⿏ࡼˈਜ⦄ߎ⬅催എⱘ䲚Ё৥Ԣഎⱘߚᬷ䍟࢓ˈѺ䇈ᯢ ডᑨᯊ䯈
݊㔥㒰㒧ᵘ㘮ড়ᑺ䰡ԢDŽ
Fig.4 Ka value and Al2O3/SiO2 ratio of fly ash

䗮䖛ᇍᬍᗻ CFA-4-1200ćⱘᤃ㤵㉝⺼໘⧚ˈ݊↨㸼䴶
Q3 4
LCFA1 Q2 Q ⿃᥻ࠊЎ 375m2/Kg ᎺেDŽ೒ 4 Ў㉝✸♄ⱘ৘啘ᳳ⌏ᗻ
Q1 Al2O3/SiO2 ↨ؐঞ ؐDŽ⬅೒ 4 ৃ㾕ˈ㒣 CFA-4-1200ć೼৘
啘ᳳⱘ ؐഛ催Ѣॳ⢊ LCFA1 ⱘˈᑊϨⳌᇍѢ LCFA1ˈ݊
ᮽᳳⱘ ؐᦤ催ᐙᑺ᳈໻ˈ1d ⱘᦤ催њ 97.94%ˈ3d ⱘᦤ催
њ 82.63%ˈ䇈ᯢ䗮䖛催⏽๲䩭ᬍᗻৢˈCFA-4-1200ćⱘ
ᮽᳳ⌏ᗻᏆᕫࠄ᳝ᬜ▔থDŽ䗮䖛݊৘啘ᳳⱘ⌏ᗻ
      
Al2O3/SiO2 ↨ ؐ ↨ 䕗 ߚ ᵤ ৃ ⶹ ˈ CFA-4-1200ć ⱘ
Q1 Al2O3/SiO2 ↨ؐ䕗Ў〇ᅮˈ෎ᴀᕬᕞѢ 66.3%ᎺেˈⳌᇍ
CFA-4-1200ć
Ѣ LCFA1 ⱘ Al2O3/SiO2 ᑇഛ↨ؐ˄㑺 31.6%˅催ߎϔ‫ס‬
໮ˈ䇈ᯢ催⏽๲䩭ⱘ䖛⿟ϡҙᇍ㉝✸♄ⱘ Si-O 䬂‫݋‬᳝⸈
ണ࡯ˈᇍ Al-O 䬂ⱘ⸈ണ࡯Ѻ᳈ࡴᯢᰒDŽ

CFA-4-0d CFA-4-7d

      ppm 

29
Fig.2 Si NMR spectra of modification fly ash

CFA-4--1d CFA-4-14d
CFA-4-1200ć

LCFA1

      ppm 

Fig.3 27Al NMR spectra of modification fly ash
Fig.5 SEM of CFA-4 at different time in K a environment
⬅೒ 5 䎳ࠡᳳⷨお[1]Ё SEM ✻⠛ᇍ↨ߚᵤৃҹথ⦄ˈ
㒣ᬍᗻৢⱘ CFA-4 ⱘ৘啘ᳳডᑨ䖛⿟Ϣॳ⢊㉝✸♄ⱘᄬ೼

5897
ᯢᰒϡৠDŽॳ⢊㉝✸♄ⱘডᑨ䖛⿟ᯢᰒ㓧᜶ˈᄬ೼㾷㘮㛑 ᦎᬍᗻ㉝✸♄ⱘ CFA3-2 ডᑨ⿟ᑺ೼৘啘ᳳ˄ᇸ݊೼
䞣ⱘ㌃⿃䖛⿟ˈ䖒ࠄϔᅮ⿟ᑺৢᠡӮ⬅㉝✸♄乫㉦㸼䴶৥ 28d Пࠡ˅ഛᯢᰒ催Ѣৠ啘ᳳⱘ FA3-2ˈᑊ೼ 14d~28d ᯊ
݊‫ݙ‬䚼䖯ϔℹডᑨˈ䖒ࠄᅠܼ㾷㘮ⱘⳂⱘ[6]DŽ㗠 CFA-4 Ң ⬅ 11.89%䎗छࠄ 16.62%ˈ䇈ᯢᬍᗻ㉝✸♄ⱘ࣪ᄺ⌏ᗻᬜ
ডᑨᓔྟˈ⺅ᗻҟ䋼ህⳈ᥹Ϣ݊㸼䴶ঞ‫ݙ‬䚼ᅠܼ᥹㾺ˈᑊ ᑨ೼ℸ䰊↉ⱘডᑨ⿟ᑺ๲ࡴ᳔ᖿˈ೼ 60d Пৢ݊ডᑨ⿟ᑺ
Ϩডᑨ䗳⥛䕗ᖿˈ೼߱ᳳህᔶ៤䕗ᯢᰒⱘࠏ㱔⦄䈵ˈ೼ ⱘ๲䭓䍟࢓ᯢᰒ‫ޣ‬㓧ˈЏ㽕ᰃ಴Ў∈࣪ѻ⠽ঞ⌚ԧᆚᅲᑺ
14d ᯊᅲ⦄ᅠܼ㾷㘮ˈᔶ៤ᵒᬷⱘẦ⢊⠽㇛ᢹԧDŽ ᦤ催䰏䱨њ։㱔ҟ䋼Ϣ㉝✸♄⌏ᗻ㒘ߚⱘ᥹㾺ˈᓊ㓧њড
ᑨ䗳⥛[10]DŽ
C. ࡯ᄺᔎᑺߚᵤ
೒ 6 Ўᦎ㉝✸♄∈⊹‫⌚ޔ‬䆩ӊᡫय़ᔎᑺDŽ⬅೒ 6 ৃ㾕ˈ E. XRD ߚᵤ
ᦎࡴᬍᗻ㉝✸♄ⱘ CFA3-2 ⱘ৘啘ᳳᡫय़ᔎᑺձ✊ԢѢ㒃 ೒ 7 Ўᦎᬍᗻᦎ㉝✸♄∈⊹‫⌚ޔ‬䆩ӊⱘ৘啘ᳳ XRD ߚ
∈⊹ԧ㋏ⱘ 0-2ˈԚⳌᇍѢ FA3-2ˈᦎࡴᬍᗻ㉝✸♄ⱘ ᵤDŽ⬅೒ 7 ৃ㾕ˈ2ș˙9.65º 䰘䖥Ў AFt ⡍ᕕዄˈᑊ䱣ⴔ啘
CFA3-2 ೼ᮽᳳ˄28d Пࠡ˅᳝ᯢᰒӬ࢓ˈϨ๲䭓䗳⥛䕗 ᳳⱘᓊ䭓ˈ݊ዄؐᯢᰒ๲ᔎDŽ2ș˙18.08º Ϣ 34.14º ໘Ў
ᖿˈ䇈ᯢᬍᗻ㉝✸♄ CFA-4 㛑᳝ᬜᬍ୘∈⊹‫ⱘ⌚ޔ‬ᮽᳳᗻ Ca(OH)2 ⱘЏ㽕⡍ᕕዄˈ݊ዄ催ৃ೼ϔᅮ⿟ᑺϞড᯴‫⌚ޔ‬
㛑[7,8]DŽⳌᇍѢ ⊩Ё⌟䆩ⱘ㒧ᵰℸ๲䭓⥛⬹ᰒϡ䎇ˈЏ㽕 ⱘ ∈ ࣪ ⿟ ᑺ DŽ ೼ ᦎ ㉝ ᬍ ᗻ ✸ ♄ ԧ ㋏ Ё ˈ CFA3-2 ⱘ
ॳ಴೼Ѣ∈⊹‫⌚ޔ‬ԧ㋏ⱘ∈࣪⦃๗Ϣ ⊩⦃๗Ⳍ↨ϡ㛑⒵䎇 Ca(OH)2 ⱘ⡍ᕕዄዄ催䱣啘ᳳⱘᓊ䭓ϔⳈਜ⦄䗦‫ޣ‬䍟࢓ˈ
ᬍᗻ㉝✸♄ CFA-4 ⱘ▔থ㽕∖ˈ಴ℸ݊࣪ᄺ⌏ᗻᬜᑨ᮴⊩
䇈ᯢᬍᗻ㉝✸♄ CFA-4 ೼∈࣪ডᑨ߱ᳳे໘Ѣᖿ䗳ডᑨ䰊
೼࡯ᄺᔎᑺᮍ䴶ᕫࠄᰒ⼎DŽ
↉ˈϡᮁ⍜㗫∈⊹ⱘ∈࣪ѻ⠽ Ca(OH)2ˈ࣪ᄺ⌏ᗻᯢᰒᦤ
催ˈ䖭Ϣ݊ᡫय़ᔎᑺⱘᮽᳳ㸼⦄Ⳍϔ㟈DŽ


 Ʒ
Ʒ Ƹ

Ƶ
ᡫ य़ ᔎ ᑺ 03D

CFA3-2-90d


 CFA3-2-60d

 CFA3-2-28d
 
)$ CFA3-2-14d
 &)$
 CFA3-2-7d
G G G G G
啘ᳳ CFA3-2-3d
Fig.6 Compressive strength of cement paste with fly ash
        
D. 䴲㪌থ∈䞣Ϣডᑨ⿟ᑺ
㸼 2 Ўᦎ㉝✸♄∈⊹‫⌚ޔ‬৘啘ᳳ䴲㪌থ∈䞣ঞ㉝✸♄ ƵˉAFt; ƷˉCa(OH)2; Ƹˉ¢-C2SH/C2S/C3S

ডᑨ⿟ᑺDŽ⬅㸼 2 ৃ㾕ˈᦎࡴᬍᗻ㉝✸♄ৢⱘ∈⊹‫⌚ޔ‬ Fig.7 XRD of cement pastes with CFA-4 at different ages
CFA3-2 ⱘ৘啘ᳳ˄ᇸ݊೼∈࣪ᮽᳳ˅䴲㪌থ∈䞣ഛ催Ѣ
㒃∈⊹‫ ⌚ޔ‬0-2 ঞ݊ᦎॳ⢊㉝✸♄ⱘ FA3-2ˈ䇈ᯢᴀ䆩偠 IV. 㒧䆎
ᴵӊϟᬍᗻ㉝✸♄ᯢᰒᦤ催њ໡ড়ԧ㋏ⱘᮽᳳ∈࣪䗳⥛ˈ 1˅㒣催⏽๲䩭ᬍᗻⱘ CFA-4 ⳌᇍѢ LCFA1 ᮽᳳⱘ
Џ㽕ॳ಴೼Ѣ㱑✊ᬍᗻ㉝✸♄ⱘ乫㉦ᔶ䉠থ⫳ᬍবˈԚᬍ K a ؐ໻ᐙᑺᦤ催ˈ䇈ᯢ CFA-4 ⱘᮽᳳ⌏ᗻᏆᕫࠄ᳝ᬜ▔
ᗻ㉝✸♄ⱘ࣪ᄺ⌏ᗻᬜᑨㄝ䍙䖛њॳ⢊㉝✸♄ⱘ乫㉦ᔶ䉠
থ DŽ CFA-4 ⱘ ⌏ ᗻ Al2O3/SiO2 ↨ ؐ Ⳍ ᇍ Ѣ LCFA1 ⱘ
‫∈ޣ‬ᬜᑨঞ࣪ᄺ⌏ᗻᬜᑨ[9]DŽ Al2O3/SiO2 ᑇഛ↨ؐ催ߎϔ‫ס‬໮ˈ䇈ᯢ催⏽๲䩭ⱘ䖛⿟ϡ
Table 2 Degree of reaction of fly ash and non-evaporable
water content of cement pastes with fly ash /% ҙᇍ㉝✸♄ⱘ Si-O 䬂‫݋‬᳝⸈ണ࡯ˈᇍ Al-O 䬂ⱘ⸈ണ࡯Ѻ
㓪ো 0-2 FA3-2 CFA3-2 ᳈ࡴᯢᰒDŽ
3d(䴲㪌থ∈䞣/ডᑨᑺ) 10.79 11.86/5.32 12.18/8.66
7d(䴲㪌থ∈䞣/ডᑨᑺ) 12.99 12.15/7.77 13.56/10.57 2˅ᬍᗻৢⱘ CFA-4 ೼ K a ⊩⦃๗ϟϡᄬ೼ࠊ㑺಴㋴
14d(䴲㪌থ∈䞣/ডᑨᑺ) 13.59 13.19/9.89 15.05/11.89 ˄े⒊㱔⌏࣪⚍ⱘߎ⦄˅ˈ݊㸼㾖⌏࣪㛑ᯢᰒ䰡ԢˈSi-O-
28d(䴲㪌থ∈䞣/ডᑨᑺ) 14.64 14.01/12.84 16.78/16.62
Al 㔥㒰㘮ড়ԧⱘ㘮ড়ᑺ䰡Ԣˈডᑨҟ䋼ৃҹᖿ䗳Ϣ㾷㘮ৢ
60d(䴲㪌থ∈䞣/ডᑨᑺ) 15.67 14.58/14.08 17.58/19.48
90d(䴲㪌থ∈䞣/ডᑨᑺ) 17.19 15.02/18.68 19.25/20.67
ⱘ SiǃAl 䖯㸠ডᑨˈ㗠ᛄᗻⱘ㥿ᴹ⷇ঞ/៪ᮄ⫳ⷓ⠽⊌⷇
ϡখϢডᑨϨ⅟ԭৢᔶ៤Ầ⢊⠽DŽ

5898
 3˅ᦎᬍᗻ㉝✸♄ԧ㋏ЁˈCFA3-2 ⱘ Ca(OH)2 ⱘ⡍ᕕዄ [3] S Antiohos I, S. Tsimas. “Investigating the role of reactive silica in the
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ᛳ䇶೑ᆊ䞡⚍෎⸔ⷨおথሩ䅵ߦ (973) ˄乍Ⳃ㓪ো˖
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