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ANEXO 1
Tabla 1. Experimentos preliminares realizados en la etapa de sembrado.
#
Concentraciones Tiempo
de agitación
Tiempo de inmersión
Tiempo de secado a alta temperatura Isopropanol Ácido clorhídrico Isopropóxido de titanio
mL moles mL moles M mL moles M min min min -°C
1 17 2.21E-01 0.04 4.53E-04 2.48E-02 1.25 4.10E-03 2.24E-01
5
30
60-120°
2 68 8.84E-01 0.16 1.81E-03 2.61E-02 1.25 4.10E-03 5.90E-02 3 51 6.63E-01 0.12 1.36E-03 2.60E-02 1.25 4.10E-03 7.82E-02 4 35 4.55E-01 0.08 9.06E-04 2.49E-02 1.25 4.10E-03 1.13E-01 5 68 8.84E-01 0.16 1.81E-03 2.61E-02 1.25 4.10E-03 5.90E-02
10 6 51 6.63E-01 0.12 1.36E-03 2.60E-02 1.25 4.10E-03 7.82E-02
7 35 4.55E-01 0.08 9.06E-04 2.49E-02 1.25 4.10E-03 1.13E-01
8 68 8.84E-01 0.16 1.81E-03 2.61E-02 1.25 4.10E-03 5.90E-02 Plasma 1 min c/lado
9 37 4.81E-01 2.08 2.36E-02 5.57E-01 3.25 1.06E-02 2.52E-01 60 - 120°
10 68 8.84E-01 0.16 1.81E-03 2.61E-02 1.25 4.10E-03 5.90E-02 Plasma 1 min cada
lado + 60’-120°
11 30
3.90E-01 0.07 7.93E-04 2.62E-02
0.25 8.19E-04 2.70E-02
5
60 - 120°
12 30 0.2 6.55E-04 2.16E-02
13 30 0.15 4.91E-04 1.63E-02
14 30 0.1 3.28E-04 1.09E-02
15 30 0.05 1.64E-04 5.44E-03
16 30 0.25 8.19E-04 2.70E-02
17 30 0.2 6.55E-04 2.16E-02
18 30 0.15 4.91E-04 1.63E-02
19 30 0.1 3.28E-04 1.09E-02
20 30 0.05 1.64E-04 5.44E-03
21 30 0.25 8.19E-04 2.70E-02
22 30 0.2 6.55E-04 2.16E-02 60 - 120° / Secado
por plasma (1min c/lado)
23 30 0.15 4.91E-04 1.63E-02
24 30 0.1 3.28E-04 1.09E-02
25 30 0.05 1.64E-04 5.44E-03
26 30 0.05 1.64E-04 5.44E-03
15 min de rampa a 140°C. 15 min de mantenimiento a 140°C. 15min de enfriamiento.
Potencia 600. Agitación (si).
27 30 0.05 1.64E-04 5.33E-03
20 min de rampa a 140°C. 20 min de mantenimiento a 140°C. 30 min de enfriamiento.
Potencia 600. Agitación (si).
28 30 0.05 1.64E-04 5.44E-03
29 30 0.15 4.91E-04 1.63E-02
30 30 0.15 4.91E-04 1.63E-02
31 30 0.1 3.28E-04 1.09E-02
32 30 0.1 3.28E-04 1.09E-02
33 30 0.05 1.64E-04 5.44E-03
34 30 0.05 1.64E-04 5.44E-03
35 60 7.80E-01 0.14 1.59E-03 2.63E-02 0.05 1.64E-04 2.72E-03 36 30
3.90E-01 0.07 7.93E-04 2.62E-02 0.15 4.91E-04 1.63E-02
37 30 2.55E-02 1 3.28E-03 1.05E-01
38 80
1.04E+00 0.185 2.09E-03 2.61E-02 0.06 1.97E-04 2.45E-03 39 80 0.2 2.27E-03 2.82E-02 0.07 2.29E-04 2.86E-03
ANEXO 2
Tabla 1. Experimentos preliminares realizados en la etapa de crecimiento.
# Condiciones (microondas)
Concentraciones
Orden de agregado
Agitació n
Tratamient o térmico Tetracloruro de titanio Ácido clorhídrico Isopropóxido de titanio
mL moles M mL moles M mL moles M min min - °C
1 30 min de rampa a 140°C. 30 min de mantenimiento a 140°C. 15 min de enfriamiento.
Potencia 600.
Agitación (si)
1 9.11E-03 3.96E-01 20 1.13E-01 4.92E+0
0 2 6.55E-03 2.85E-01
HCl. fibras.
Isopropóxid o de Ti.
Tetracloruro de Ti
5
0
2 0.5 4.55E-03 2.74E+00 0.16 9.06E-04 5.46E-01 1 3.28E-03 1.97E+0 0
3 30 min de rampa a 80°C. 30 min de mantenimiento a 100°C. 15 min de enfriamiento.
Potencia 600.
Agitación (si)
0.25 2.28E-03 5.59E-02 40 2.27E-01 5.56E+0
0 0.5 1.64E-03 4.02E-02 4 0.15 1.37E-03 3.38E-02 40 2.27E-01 5.60E+0
0 0.3 9.83E-04 2.43E-02 5 30 min de rampa a
140°C. 30 min de mantenimiento a 140°C. 15 min de enfriamiento.
Potencia 600.
Agitación (si)
0.5 4.55E-03 2.12E-01 20 1.13E-01 5.27E+0
0 1 3.28E-03 1.52E-01
1h-120
6 0.25 2.28E-03 1.10E-01 20 1.13E-01 5.46E+0
0 0.5 1.64E-03 7.89E-02 7 0.2 1.82E-03 8.84E-02 20 1.13E-01 5.50E+0
0 0.4 1.31E-03 6.36E-02
HCl.
Isopropóxid o de Ti.
Tetracloruro de Ti. fibra
0
8 0.1 9.11E-04 4.49E-02 20 1.13E-01 5.58E+0
0 0.2 6.55E-04 3.23E-02 9 10 min de rampa a
80°C (Potencia 200).
Sostenimiento a 80°C 5 min. 50 min de rampa a 140°C.
10 min de
mantenimiento a 140°C. 10 min de rampa a 140 y 10
min de
sostenimiento a 140.
Potencia 600.
Agitación (si)
0.45 4.10E-03 1.92E-01 20 1.13E-01 5.31E+0
0 0.9 2.95E-03 1.38E-01
10 0.35 3.19E-03 1.51E-01 20 1.13E-01 5.38E+0
0 0.7 2.29E-03 1.09E-01