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*        : Dongbai Zhang, Limin Qi, Jiming Ma and Humin Cheng
* !"#$%"&'() $* + ก--(.(&$ก/$ (0# !"#$%"12กก3 1-*&!+4)5
* &$(!)3 14 89%9!)3 1 05# 100-103 1= 2003
* ?@-%9-# %$ : 18 ก-กB#'( 2002
* -%9-C (# -D#5 : 9 /$#'( 2002
* )F(FG'-%H -ก : 29 /$#'( 2002
ก#-I% &'-#*0G $Jก?!!#&5)"(?@CCก?K@G (TiO2) .@"ก#-I$#" % PC ?!!#&5)"(
&! -*9CCก?K@G (titanium Tetrabutoxide) ก%9ก-@?T.@-'$C-กU5 NP-5 (Igepal CO-520)/
Cyclohexane !)3C/_0`(0C @ " a) Reverse Micelle .@"U0?@C5/`#'9-I/!ae!)3()
.'- I-# 99 Rutile U5I`# *' #(&1f5ก-@!)3&0(#*I(
    1244%"!)3() $ C1gก-"# 'hC
           - ' #(&P(P5PC ก-@
           - '#' !)3PC 5Hi# (w=[H2O]/[NP-5])
KJ3 4*&1f5 $ C$%กn_*!# I%_D#5 !"# !%H &oIPC $Jก $*P5#@C5/`#'PC $Jก
?!!#&5)"(?@CCก?K@G (TiO2) I@ U0&0p5qJ &Iq)"-`#F!# &'()I &r5()'#@%r5)ก#--
0%ก&0 C I $*'#' !)3C&$pก!-ก KJ3 ()9!9#!Ii#'%s CI#P# r#Ch35
   U51=!)3 #5(#$#I/@()ก#-&F3(' #(I5U4U5ก#-1-*"/ก C5/`#'?!!#&5)"(?@CCก?K@G
                                                    G
(TiO2) &Fh3C!i#&(p@I)&- 1gก-"# I5%9I5/5ก#-UrU5 &K-#(ก กt#K &Kp5&KC-G I#-&'$hC9!# -
&'() !i#U05Hi#9-I/!ae $* F$% #5&K$$G I C#! "G &1f5 5
   ก#-5i#?11-*"/ก GUr5%H5 .'- I-# PC $Jก5%H5() $C"# (#ก @% 5%H54J 4i#&1f5C"# "3 !)3
4* C ()ก#-I% &'-#*0G?!!#&5)"(?@CCก?K@G (TiO2) U0?@.'- I-# PC C5/`#'U5-*@%9
5#.5 .@"&-#I#(#-q' 9'/(?@ % C"# ก#-I% &'-#*0G 99 a)&@( &r5 ก-*9 5ก#-K%5&o
ก#-9 5ก#-.K$&4$ $*ก#-' 9 55
( )
   &(h3C&-p u 5)H()ก#-5i# a)ก#- Reverse Micelle 5i#?1UrU5ก#-I% &'-#*0GC5/`#'5#.5PC
?!!#&5)"(?@CCก?K@G (TiO2) .@"()I#-r "$@ - J
   ก-*9 5ก#- Reverse Micelle ()PC?@&1-)"9C"# (#กก%9ก#-I% &'-#*0GI#-U59CC5/`#'
.@"ก#-9 5ก#-5)H() 5 '@ 'hC ก#- F-PC I#- 99 microreactors !)3&0(#*I( U5ก#-
I% &'-#*0GC5/`#'5#.5 a)5)HC5/`#'!)3?@"% ()' #(rhH5C"4J qก4i#4%@U5!# 1g9%
ก

- I#-$@ - J NP-5 (Igepal CO-520) , Mn 441
- ?!!#&5)"(&! -*9CCก?K@G (titanium Tetrabutoxide)
- ?K.'$&Tก&K5 (cyclohexane) , C6H12
- ก-@?T.@-'$C-ก (hydrochloric)
- 5Hi#ก$%35
ก
                                                          [ Titanium Tetrabutoxide + (Cyclohexane, C6H12 )]
    ก              ก (HCl), 73 uL, 2.5 M
                                                                          135 uL, 1.25 M

[( NP-5/H2O, w = 8) + ( Cyclohexane, C6H12 )]
                                                                     [h = (H2O)/(Ti(OC4H9)4)] = 28
               5 mL, 0.15 M
                 Oil phase                                                 Water phase
                                           H 5, 10, 20   IJ KLMNO 22 °c


                                   H   H ethanol H Q RJ centrifuged
                                             IJ 3000 / I


                                  TEM                              XRD
(a.1)   (b.1)




(c.1)
                     &!'5' TEM &FhC+Jกn#$%กn_*I%_D#5 !"#
                                    3
                PC C5/`#' TiO2 w = 5 , h = 28
                     กi#05@' #(&P(P5PC ก-@?T.@-'$C-ก(HCl)
                  # u@% 5)H
                (a.1) = 1.5 mol/L (C5/`#'().'- I-# ?(I(3#&I(C)
                                                          i
                (b.1) = 2.0 mol/L (C5/`#' 99 rutile pure+anatase)
                (c.1) = 2.5 mol/L (C5/`#' 99 rutile pure)
XRD   M TiO2,w = 5, h = 28, 2.5 mol/L


                         P5#@PC $Jก lattice parameter
                              3.209 °A = (110)
                              2.467 °A = (101)
                              2.259 °A = (200)
                              1.670 °A = (211)
                              1.470 °A = (002)
                              1.397 °A = (301)
+Jกn#C!aF$PC 5Hi#
ก-@?T.@-'$C-ก 2.5 M, h ([H2O]/[Ti(OC4H9)4]) =8, 20 %5




                (a.2) w = 3                                  (b.2) w = 10
    C5/`#'().'- I-# 99 rutile ก-*4#" % ()      C5/`#'()ก#-- ( % ก%5'$#"uก$%9@Cก?( ()
$%กn_*'$#"u-q"5 G ' #(ก # ()P5#@1-*(#_      .'- I-# 99 rutile $* anatase ก#-I-# $Jก
35-40                               150-    4*0"/@&(h3C1-(# -PC 5Hi#(#กu (w I )
160
+Jกn#C!aF$PC C% -#I 5-*0 # H2O/Ti
ก-@?T.@-'$C-ก 2.5 M, w = 8, 20 %5


                                             (a.3) h = 10
                                             (b.3) h = 20
                                             (c.3) h = 36
                                        &(h3CC% -#I 5-*0 #
                                    H2O/Ti &F3((#กPJH5 h >10
                                    C5/`#'()ก#-&1f5.'- I-#
                                     $*$%กn_*'$#"ก$)9
                                    @Cก?( $*()ก#-4%9ก$/(
                                    - ( % ก%5(#กPJH5
+Jกn#C!aF$PC ก-@
' #(&P(P5PC ก-@!@IC9 2.5 M, w = 8 h ([H2O]/[Ti(OC4H9)4]) = 8, 20 %5

                                                               (a.4) ก-@?5 -ก C5/`#'()
                                                                     ก       20-25

                                                                       120
                                                               (b.4) ก-@ ! "ก #
                                                                    $ % &' (! )ก
                                                                        40
                                                               (c.4) ก-@ % % #
                                                                    $*+,'- ก -#. #
                                                                % &' (! ก)
                                                               240
+Jกn#C!aF$PC & $#
ก-@?T.@-'$C-ก 2.5 M, w = 8, h = 8

                                       (a.5) 5 %5 C5/`#'&-3(
                                       & 9. $*4%9 % ก%5&1f5()
                                       ก#-ก-*4#" % PC C5/`#'
                                       ' #(ก # 30
                                                          120
                                               กC5
                                       (b.5) 10 %5 &-3(- " % 4%9
                                       ก%5'$#"ก$)9@Cก?(
                                       (c.5) 20 %5 C5/`#'4%9 %
                                       ก%5&1f5@Cก?(C"# I(9-_G
I-/1
    ก#-I% &'-#*0GC5/`#'5#.5PC I#-?!&!&5)"(?@CCก?K@G (TiO2) KJ3 & h3C5?P!)3()
$ C1gก-"#ก#-I-# $JกU0().'- I-# pure rutile #5ก-*9 5ก#- Reverse Micelle
C C"U5C/_0`(0C $*()I`# *' #(&1f5ก-@!)3&0(#*I(

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การสังเคราะห์ผลึกไททาเนียมไดออกไซด์

  • 1. * : Dongbai Zhang, Limin Qi, Jiming Ma and Humin Cheng * !"#$%"&'() $* + ก--(.(&$ก/$ (0# !"#$%"12กก3 1-*&!+4)5 * &$(!)3 14 89%9!)3 1 05# 100-103 1= 2003 * ?@-%9-# %$ : 18 ก-กB#'( 2002 * -%9-C (# -D#5 : 9 /$#'( 2002 * )F(FG'-%H -ก : 29 /$#'( 2002
  • 2. ก#-I% &'-#*0G $Jก?!!#&5)"(?@CCก?K@G (TiO2) .@"ก#-I$#" % PC ?!!#&5)"( &! -*9CCก?K@G (titanium Tetrabutoxide) ก%9ก-@?T.@-'$C-กU5 NP-5 (Igepal CO-520)/ Cyclohexane !)3C/_0`(0C @ " a) Reverse Micelle .@"U0?@C5/`#'9-I/!ae!)3() .'- I-# 99 Rutile U5I`# *' #(&1f5ก-@!)3&0(#*I( 1244%"!)3() $ C1gก-"# 'hC - ' #(&P(P5PC ก-@ - '#' !)3PC 5Hi# (w=[H2O]/[NP-5]) KJ3 4*&1f5 $ C$%กn_*!# I%_D#5 !"# !%H &oIPC $Jก $*P5#@C5/`#'PC $Jก
  • 3. ?!!#&5)"(?@CCก?K@G (TiO2) I@ U0&0p5qJ &Iq)"-`#F!# &'()I &r5()'#@%r5)ก#-- 0%ก&0 C I $*'#' !)3C&$pก!-ก KJ3 ()9!9#!Ii#'%s CI#P# r#Ch35 U51=!)3 #5(#$#I/@()ก#-&F3(' #(I5U4U5ก#-1-*"/ก C5/`#'?!!#&5)"(?@CCก?K@G G (TiO2) &Fh3C!i#&(p@I)&- 1gก-"# I5%9I5/5ก#-UrU5 &K-#(ก กt#K &Kp5&KC-G I#-&'$hC9!# - &'() !i#U05Hi#9-I/!ae $* F$% #5&K$$G I C#! "G &1f5 5 ก#-5i#?11-*"/ก GUr5%H5 .'- I-# PC $Jก5%H5() $C"# (#ก @% 5%H54J 4i#&1f5C"# "3 !)3 4* C ()ก#-I% &'-#*0G?!!#&5)"(?@CCก?K@G (TiO2) U0?@.'- I-# PC C5/`#'U5-*@%9 5#.5 .@"&-#I#(#-q' 9'/(?@ % C"# ก#-I% &'-#*0G 99 a)&@( &r5 ก-*9 5ก#-K%5&o ก#-9 5ก#-.K$&4$ $*ก#-' 9 55
  • 4. ( ) &(h3C&-p u 5)H()ก#-5i# a)ก#- Reverse Micelle 5i#?1UrU5ก#-I% &'-#*0GC5/`#'5#.5PC ?!!#&5)"(?@CCก?K@G (TiO2) .@"()I#-r "$@ - J ก-*9 5ก#- Reverse Micelle ()PC?@&1-)"9C"# (#กก%9ก#-I% &'-#*0GI#-U59CC5/`#' .@"ก#-9 5ก#-5)H() 5 '@ 'hC ก#- F-PC I#- 99 microreactors !)3&0(#*I( U5ก#- I% &'-#*0GC5/`#'5#.5 a)5)HC5/`#'!)3?@"% ()' #(rhH5C"4J qก4i#4%@U5!# 1g9%
  • 5. ก - I#-$@ - J NP-5 (Igepal CO-520) , Mn 441 - ?!!#&5)"(&! -*9CCก?K@G (titanium Tetrabutoxide) - ?K.'$&Tก&K5 (cyclohexane) , C6H12 - ก-@?T.@-'$C-ก (hydrochloric) - 5Hi#ก$%35
  • 6. [ Titanium Tetrabutoxide + (Cyclohexane, C6H12 )] ก ก (HCl), 73 uL, 2.5 M 135 uL, 1.25 M [( NP-5/H2O, w = 8) + ( Cyclohexane, C6H12 )] [h = (H2O)/(Ti(OC4H9)4)] = 28 5 mL, 0.15 M Oil phase Water phase H 5, 10, 20 IJ KLMNO 22 °c H H ethanol H Q RJ centrifuged IJ 3000 / I TEM XRD
  • 7. (a.1) (b.1) (c.1) &!'5' TEM &FhC+Jกn#$%กn_*I%_D#5 !"# 3 PC C5/`#' TiO2 w = 5 , h = 28 กi#05@' #(&P(P5PC ก-@?T.@-'$C-ก(HCl) # u@% 5)H (a.1) = 1.5 mol/L (C5/`#'().'- I-# ?(I(3#&I(C) i (b.1) = 2.0 mol/L (C5/`#' 99 rutile pure+anatase) (c.1) = 2.5 mol/L (C5/`#' 99 rutile pure)
  • 8. XRD M TiO2,w = 5, h = 28, 2.5 mol/L P5#@PC $Jก lattice parameter 3.209 °A = (110) 2.467 °A = (101) 2.259 °A = (200) 1.670 °A = (211) 1.470 °A = (002) 1.397 °A = (301)
  • 9. +Jกn#C!aF$PC 5Hi# ก-@?T.@-'$C-ก 2.5 M, h ([H2O]/[Ti(OC4H9)4]) =8, 20 %5 (a.2) w = 3 (b.2) w = 10 C5/`#'().'- I-# 99 rutile ก-*4#" % () C5/`#'()ก#-- ( % ก%5'$#"uก$%9@Cก?( () $%กn_*'$#"u-q"5 G ' #(ก # ()P5#@1-*(#_ .'- I-# 99 rutile $* anatase ก#-I-# $Jก 35-40 150- 4*0"/@&(h3C1-(# -PC 5Hi#(#กu (w I ) 160
  • 10. +Jกn#C!aF$PC C% -#I 5-*0 # H2O/Ti ก-@?T.@-'$C-ก 2.5 M, w = 8, 20 %5 (a.3) h = 10 (b.3) h = 20 (c.3) h = 36 &(h3CC% -#I 5-*0 # H2O/Ti &F3((#กPJH5 h >10 C5/`#'()ก#-&1f5.'- I-# $*$%กn_*'$#"ก$)9 @Cก?( $*()ก#-4%9ก$/( - ( % ก%5(#กPJH5
  • 11. +Jกn#C!aF$PC ก-@ ' #(&P(P5PC ก-@!@IC9 2.5 M, w = 8 h ([H2O]/[Ti(OC4H9)4]) = 8, 20 %5 (a.4) ก-@?5 -ก C5/`#'() ก 20-25 120 (b.4) ก-@ ! "ก # $ % &' (! )ก 40 (c.4) ก-@ % % # $*+,'- ก -#. # % &' (! ก) 240
  • 12. +Jกn#C!aF$PC & $# ก-@?T.@-'$C-ก 2.5 M, w = 8, h = 8 (a.5) 5 %5 C5/`#'&-3( & 9. $*4%9 % ก%5&1f5() ก#-ก-*4#" % PC C5/`#' ' #(ก # 30 120 กC5 (b.5) 10 %5 &-3(- " % 4%9 ก%5'$#"ก$)9@Cก?( (c.5) 20 %5 C5/`#'4%9 % ก%5&1f5@Cก?(C"# I(9-_G
  • 13. I-/1 ก#-I% &'-#*0GC5/`#'5#.5PC I#-?!&!&5)"(?@CCก?K@G (TiO2) KJ3 & h3C5?P!)3() $ C1gก-"#ก#-I-# $JกU0().'- I-# pure rutile #5ก-*9 5ก#- Reverse Micelle C C"U5C/_0`(0C $*()I`# *' #(&1f5ก-@!)3&0(#*I(