[ 화학 ] 과학고 R&E 결과보고서 속이빈무기물나노입자제조법연구 연구기간 : 2013. 4. 1 ~ 2013. 12. 31 연구책임자 : 류광선 ( 울산대화학전공 ) 지도교사 : 이한섭 ( 울산과학고유기화학과 ) 참여학생 : 설혜경 ( 울산과학고 1학년 ) 모현영 ( 울산과학고 1학년 ) 김도영 ( 울산과학고 1학년 ) 문지원 ( 울산과학고 1학년 ) 김태민 ( 울산과학고 1학년 )
1 1.
[ ] - -, [ ] - - (SiO 2 ) - NH 4 OH 0.4M ( : ) 1:0, 1:1, 0:1 - ( : ) 1:0 NH 4 OH (1.0M, 1.5M, 2.0M) - - XRD, FE-SEM, FT-IR [ - ] - - - (, ) - - (1.0M, 2.0M) -
- XRD, FE-SEM, FE-TEM, FT-IR [ ] - NaOH (1.0M, 2.0M), - XRD, FE-SEM, FE-TEM, FT-IR -,, [ ] - - -, 3. 1. SiO 2 SiO 2. ethanol n-propanol. ethanol 250nm SiO 2, n-propanool 400~700nm SiO 2, aggregation. Methanol(polarity index 6.6) SiO 2, Diethyl ether(polarity index 2.8).., 6.4M. 6.4M 300nm SiO 2. 3.2M 1.6M. SiO 2. 1 ethanol SiO 2, 6.4M. 3. 2. SiO 2 -TiO 2 core-shell, TEM TiO 2, aggregation, SiO 2 @TiO 2 core-shell. acetic acid, isoproyl alcohol TTIP H2O
SiO2., TiO 2 SiO 2- TiO2 core-shell TiO 2 SiO 2. TiO 2, XRD, SEM, TEM SiO 2 TiO 2 ( 10nm ). 3. 3. TiO 2 hollow-shell NaOH TiO 2 hollow network. 1N 2N NaOH 2N NaOH, SiO 2, TIO 2 hollow network. TiO 2 hollow network 2. [ ] - - - - - -, [ ] -
ethanol 200nm SiO 2, 6.4M. SiO 2 -TiO 2 core-shell TiO 2 ( 10nm ) core-shell, 2N NaOH, SiO 2 TiO 2 hollow-network.
Ⅰ.... 10 1. 1 1 10 1 1 100 1. 1, 1nm 10 1.,,,.,,,,,.,,,,,,, -,,,.,.,. Ⅱ. 연구방법및이론 1. 여러가지조건에따른 SiO 2 의합성. SiO 2 (1) Methanol(polarity index 6.6), Ethanol(polarity index 5.2), N-propanol(polarity index 4), Diethyl ether(polarity index 2.8). SiO 2, SiO 2. [Si(OC 2H 5) 4 + 2H 2O SiO 2 + 4C 2H 5OH] < > (2) 1 0.2M Tetraethyl orthosilicate (TEOS) 9.10ml 100ml. 2 NH4OH(16.92ml) H2O 1.2ml 100ml. 3 1. 4 12.
< SiO 2 > 5. < > 6 (SiO 2 ). 7. 8 100 24 SiO 2.
. SiO 2 (1) Ethanol, NH 4 OH 6.4M, 3.2M, 1.6M. (2) 1 0.2M Tetraethyl orthosilicate (TEOS) 9.10ml ethanol 100ml. 2 NH 4OH(16.92ml) H 2O 1.2ml ethanol 100ml. 3 1.
4 12. 5. 6 (SiO 2 ). 7. 8 100 24 SiO 2. 2. SiO 2 /TiO 2 core-shell. SiO 2 /TiO 2 core-shell (1) acetic acid 1M, isopropyl alcohol : ethanol 1 1 : 0 2 1 : 1 3 0 : 1. SiO 2 /TiO 2 core-shell. Ti(OC 2H 5) 4+4H 2O+( ) -> Ti(OH) 4+4C 2H 5OH Ti(OH) 4 + ( )->TiO 2 +2H 2 O
SiO 2 TTIP SiO 2 TiO 2. (2) 1 SiO 2 isopropyl alcohol. 2 TTIP(Titanium(IV) isopropoxide) acetic acid isoproyl alcohol. 3 SiO 2 suspension.
4 100. 5 500 3. 6 SiO 2@TiO 2.. SiO 2/TiO 2 core-shell, (1) ethyl cellulose Ethanol : methanol 1 : 0 (20ml :0ml), 1 : 1 (10ml:10ml). SiO 2 Ethanol. Ethanol, 90 0 Rutile- TiO 2. SiO 2 /TiO 2 core-shell. SiO 2 TTIP SiO 2 TiO 2.
(2) 1 SiO 2 0.3g 20ml 10. 2 ethyl cellulose 1g/L (0.04g) (1ml). 3 TTIP(1ml) (20ml). 4 3. 5 8. 6 45 o C. 7 900 o C 3. 8 SiO 2@TiO 2. 3. SiO 2 /TiO 2 core-shell. NaOH TiO 2 hollow-shell (1) SiO 2 NaOH 1N, 2N. SiO 2 SiO 2 + 2NaOH H 2O + Na 2SiO 3. Na 2SiO 3, TiO 2. (2) 1 SiO 2 @TiO 2 0.5g NaOH 50ml.
2 8 100. Ⅲ. 1. SiO 2. SiO 2 (1) XRD
<XRD > <SiO 2 > (2) FE-SEM - Ethanol. 250nm. - N-propanol. 400~700nm Ethanol. (aggregation ).
- Methanol(polarity index 6.6), Diethyl ether(polarity index 2.8).. SiO 2 (1) - NH 4 OH 6.4M SiO 2 3.2M, 1.6M. SiO 2.. (2) FE-SEM - NH 4OH 6.4M FE-SEM.
300nm. 2. SiO 2 /TiO 2 core-shell. SiO 2/TiO 2 core-shell (1) XRD isopropyl alcohol 1 : ehanol 0 isopropyl alcohol 1 : ethanol 1 isopropyl alcohol 0 : ethanol 1 Intensity (a.u.) 20 30 40 50 60 70 80 2theta < XRD > < > - XRD, SiO 2/TiO 2 core-shell.
- TiO 2,. SiO 2@TiO 2 core-shell... SiO 2 /TiO 2 core-shell, (1) XRD < XRD > < > - 900 SiO2-rutile TiO2 core-shell TiO 2 intensity. (2) SEM - SiO 2, SiO 2 TiO 2., SiO 2 /TiO 2 core-shell.
(3) EDS - Ethanol : methanol 1 1 : 0 (20ml :0ml) - Ethanol : methanol 2 1 : 1 (10ml :10ml) Si Ti. (4) FE-TEM - (10nm ).
3. SiO 2 /TiO 2 core-shell. NaOH SiO 2 /TiO 2 core-shell (1) SEM <1N NaOH > <2N NaOH > - 1N NaOH SiO 2, 2N NaOH SiO 2. SiO 2 TiO 2 network( ) (2) EDS 1 1N NaOH 2 2N NaOH - EDS NaOH SiO 2,
., core-shell Si hollow-shell Si. SiO 2. Ⅳ. 1. SiO 2 SiO 2. ethanol n-propanol. ethanol 250nm SiO 2, n-propanool 400~700nm SiO 2, aggregation. Methanol(polarity index 6.6) SiO 2, Diethyl ether(polarity index 2.8).., 6.4M. 6.4M 300nm SiO 2. 3.2M 1.6M. SiO 2. 1 ethanol SiO 2, 6.4M. 2. SiO 2-TiO 2 core-shell, TEM TiO 2, aggregation, SiO 2 @TiO 2 core-shell. acetic acid, isoproyl alcohol TTIP H2O SiO2., TiO 2 SiO 2- TiO2 core-shell TiO 2 SiO 2. TiO 2, XRD, SEM, TEM SiO 2 TiO 2 ( 10nm ). 3. TiO 2 hollow-shell NaOH TiO 2 hollow network. 1N 2N NaOH 2N NaOH, SiO 2, TIO 2 hollow network. TiO 2 hollow network 2. Ⅴ.