Chinese Journal of Catalysis ›› 2024, Vol. 59: 303-323.DOI: 10.1016/S1872-2067(24)60010-0
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Dae-Hwan Lima, Aadil Bathlaa, Hassan Anwerb, Sherif A. Younisa,c, Danil W. Boukhvalovd,e, Ki-Hyun Kima,*()
Received:
2024-01-16
Accepted:
2024-02-14
Online:
2024-04-18
Published:
2024-04-15
Contact:
*E-mail: Dae-Hwan Lim, Aadil Bathla, Hassan Anwer, Sherif A. Younis, Danil W. Boukhvalov, Ki-Hyun Kim. The effects of nitrogen-doping on photocatalytic mineralization of TiO2 nanocatalyst against formaldehyde in ambient air[J]. Chinese Journal of Catalysis, 2024, 59: 303-323.
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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(24)60010-0
Order | Code | N/Ti molar ratio (sample code: N) | TiO2 concentration in solution (sample code: C, mg mL-1) | Volume of solution (mL) | Loading mass onto the HC filter (mg) |
---|---|---|---|---|---|
1 | AP (N0-C1) | 0 | 1 | 523 | 24.2 |
2 | AP (N0-C5) | 5 | 209 | 46.5 | |
3 | AP (N0-C10) | 10 | 105 | 57.4 | |
4 | AP (N0-C20) | 20 | 52.3 | 85.1 | |
5 | AP (N1-C1) | 1 | 1 | 523 | 25.1 |
6 | AP (N1-C5) | 5 | 209 | 45.4 | |
7 | AP (N1-C10) | 10 | 105 | 56.3 | |
8 | AP (N1-C20) | 20 | 52.3 | 87.2 | |
9 | AP (N5-C1) | 5 | 1 | 523 | 25.7 |
10 | AP (N5-C5) | 5 | 209 | 47 | |
11 | AP (N5-C10) | 10 | 105 | 59.2 | |
12 | AP (N5-C20) | 20 | 52.3 | 87.3 | |
13 | AP (N10-C1) | 10 | 1 | 523 | 25.6 |
14 | AP (N10-C5) | 5 | 209 | 47 | |
15 | AP (N10-C10) | 10 | 105 | 59.9 | |
16 | AP (N10-C20) | 20 | 52.3 | 88.3 | |
17 | AP (N20-C10) | 20 | 10 | 105 | 58.8 |
Table 1 List of N-TiO2 filters prepared for the construction of AP systems. The code for each catalyst filter has been assigned in relation to the synthesis conditions and loading mass on the ceramic honeycomb (HC) filter.
Order | Code | N/Ti molar ratio (sample code: N) | TiO2 concentration in solution (sample code: C, mg mL-1) | Volume of solution (mL) | Loading mass onto the HC filter (mg) |
---|---|---|---|---|---|
1 | AP (N0-C1) | 0 | 1 | 523 | 24.2 |
2 | AP (N0-C5) | 5 | 209 | 46.5 | |
3 | AP (N0-C10) | 10 | 105 | 57.4 | |
4 | AP (N0-C20) | 20 | 52.3 | 85.1 | |
5 | AP (N1-C1) | 1 | 1 | 523 | 25.1 |
6 | AP (N1-C5) | 5 | 209 | 45.4 | |
7 | AP (N1-C10) | 10 | 105 | 56.3 | |
8 | AP (N1-C20) | 20 | 52.3 | 87.2 | |
9 | AP (N5-C1) | 5 | 1 | 523 | 25.7 |
10 | AP (N5-C5) | 5 | 209 | 47 | |
11 | AP (N5-C10) | 10 | 105 | 59.2 | |
12 | AP (N5-C20) | 20 | 52.3 | 87.3 | |
13 | AP (N10-C1) | 10 | 1 | 523 | 25.6 |
14 | AP (N10-C5) | 5 | 209 | 47 | |
15 | AP (N10-C10) | 10 | 105 | 59.9 | |
16 | AP (N10-C20) | 20 | 52.3 | 88.3 | |
17 | AP (N20-C10) | 20 | 10 | 105 | 58.8 |
Order | Sample code* | BET surface area (SBET, m2 g-1) | Pore volume (Vt, cm3 g-1) | Average pore diameter (dp, nm) | Crystallite size (nm) | Bandgap energy (eV) | Photocurrent density (μA cm-2) |
---|---|---|---|---|---|---|---|
1 | AP (N0-C10) | 75.1 | 0.184 | 7.39 | 11.1 | 3.25 | 25.8 |
2 | AP (N1-C10) | 59.2 | 0.100 | 5.25 | 10.6 | 3.10 | 29.4 |
3 | AP (N5-C10) | 62.6 | 0.121 | 5.77 | 10.4 | 3.10 | 33.8 |
4 | AP (N10-C10) | 64.4 | 0.105 | 4.79 | 10.0 | 3.10 | 45.4 |
Table 2 Physical characteristics of AP systems built using diverse forms of N-TiO2 filters (e.g., AP (N0-C10), AP (N1-C10), AP (N5-C10), and AP (N10-C10)).
Order | Sample code* | BET surface area (SBET, m2 g-1) | Pore volume (Vt, cm3 g-1) | Average pore diameter (dp, nm) | Crystallite size (nm) | Bandgap energy (eV) | Photocurrent density (μA cm-2) |
---|---|---|---|---|---|---|---|
1 | AP (N0-C10) | 75.1 | 0.184 | 7.39 | 11.1 | 3.25 | 25.8 |
2 | AP (N1-C10) | 59.2 | 0.100 | 5.25 | 10.6 | 3.10 | 29.4 |
3 | AP (N5-C10) | 62.6 | 0.121 | 5.77 | 10.4 | 3.10 | 33.8 |
4 | AP (N10-C10) | 64.4 | 0.105 | 4.79 | 10.0 | 3.10 | 45.4 |
Fig. 1. SEM images of AP HC-Nx-TiO2 photocatalytic systems: AP (N0-C10) (a), AP (N1-C10) (b), AP (N5-C10) (c), AP (N10-C10) (d), and EDS mapping of AP (N10-C10) (e-h).
Fig. 3. The XPS spectra of N-TiO2 photocatalysts (e.g., AP (N0-C10), AP (N1-C10), AP (N5-C10), and AP (N10-C10)). (a) full XPS scan; (b) Ti 2p; (c) O 1s; (d) N 1s signals.
Fig. 4. The optical properties of AP (Nx-C10; x = 0, 1, 5, 10, and 20) filters. (a) UV-vis DRS spectra; (b) Tauc plots (band gap energy); (c) PL spectra; (d) TRPL spectra.
Fig. 6. Removal efficiency of FA (5 ppm) onto AP (Nx-Cy) photocatalytic filters under combinatorial effects of Nx (0-10) and Cy (2-20 mg mL-1) under UV-LED light (a) and AP (Nx-C10; x = 0, 10, and 20) in dark vs. UV-LED light conditions (b).
A. Types of photocatalytic filter | ||||||
---|---|---|---|---|---|---|
Order | Composites | Decay rate (min-1) | R2 | CADR (L min-1) | RE (%) | |
1 | AP (blank) | 0.01 | 0.9168 | —a | — a | |
2 | AP (N0-C2) | 0.24 | 0.8944 | 3.99 | 66.0 | |
3 | AP (N0-C5) | 0.35 | 0.9663 | 5.78 | 80.6 | |
4 | AP (N0-C10) | 0.45 | 0.9286 | 7.56 | 87.0 | |
5 | AP (N0-C20) | 0.58 | 0.98 | 9.62 | 93.2 | |
6 | AP (N1-C2) | 0.28 | 0.9442 | 4.63 | 72.4 | |
7 | AP (N1-C5) | 0.42 | 0.9712 | 7.02 | 86.4 | |
8 | AP (N1-C10) | 0.53 | 0.9711 | 8.83 | 91.4 | |
9 | AP (N1-C20) | 0.60 | 0.9819 | 10.0 | 94.0 | |
10 | AP (N5-C2) | 0.31 | 0.9316 | 5.06 | 75.4 | |
11 | AP (N5-C5) | 0.43 | 0.9596 | 7.16 | 87.0 | |
12 | AP (N5-C10) | 0.55 | 0.9771 | 9.17 | 92.4 | |
13 | AP (N5-C20) | 0.61 | 0.9351 | 10.3 | 94.2 | |
14 | AP (N10-C2) | 0.34 | 0.9256 | 5.55 | 78.4 | |
15 | AP (N10-C5) | 0.45 | 0.9351 | 7.45 | 87.6 | |
16 | AP (N10-C10) | 0.57 | 0.9782 | 9.45 | 93.0 | |
17 | AP (N10-C20) | 0.64 | 0.936 | 10.7 | 95.0 | |
18 | AP (N20-C10) | 0.54 | 0.9769 | 9.00 | 91.6 | |
B. Effect of operation variables on the AP (N10-C10) photocatalytic performance | ||||||
Order | Parameter | Decay rate (min-1) | R2 | CADR (L min-1) | RE (%) | |
(1) FA concentration (ppm) | ||||||
19 | 0.5 | 1.14 | 0.9795 | 19.1 | 100 | |
20 | 1 | 0.80 | 0.9792 | 13.5 | 98.0 | |
21 | 3 | 0.67 | 0.9666 | 11.2 | 95.3 | |
22 | 5 | 0.57 | 0.9782 | 9.45 | 93.0 | |
(2) AP flow rate (L min-1) | ||||||
23 | 100 | 0.52 | 0.9943 | 8.73 | 92.0 | |
24 | 130 | 0.54 | 0.9901 | 9.07 | 92.6 | |
25 | 160 | 0.57 | 0.9782 | 9.45 | 93.0 | |
(3) Gas humidity (RH, %) | ||||||
26 | 0 | 0.57 | 0.9782 | 9.45 | 93.0 | |
27 | 20 | 0.31 | 0.9967 | 5.10 | 79.0 | |
28 | 50 | 0.21 | 0.9948 | 3.33 | 64.6 | |
29 | 100 | 0.14 | 0.983 | 2.24 | 49.6 |
Table 3 Photocatalytic performance analysis of the engineered AP (Nx-Cy) filters for FA removal under varying conditions based on the decay rate constants (k), CADR, and removal efficiency (RE%) criteria.
A. Types of photocatalytic filter | ||||||
---|---|---|---|---|---|---|
Order | Composites | Decay rate (min-1) | R2 | CADR (L min-1) | RE (%) | |
1 | AP (blank) | 0.01 | 0.9168 | —a | — a | |
2 | AP (N0-C2) | 0.24 | 0.8944 | 3.99 | 66.0 | |
3 | AP (N0-C5) | 0.35 | 0.9663 | 5.78 | 80.6 | |
4 | AP (N0-C10) | 0.45 | 0.9286 | 7.56 | 87.0 | |
5 | AP (N0-C20) | 0.58 | 0.98 | 9.62 | 93.2 | |
6 | AP (N1-C2) | 0.28 | 0.9442 | 4.63 | 72.4 | |
7 | AP (N1-C5) | 0.42 | 0.9712 | 7.02 | 86.4 | |
8 | AP (N1-C10) | 0.53 | 0.9711 | 8.83 | 91.4 | |
9 | AP (N1-C20) | 0.60 | 0.9819 | 10.0 | 94.0 | |
10 | AP (N5-C2) | 0.31 | 0.9316 | 5.06 | 75.4 | |
11 | AP (N5-C5) | 0.43 | 0.9596 | 7.16 | 87.0 | |
12 | AP (N5-C10) | 0.55 | 0.9771 | 9.17 | 92.4 | |
13 | AP (N5-C20) | 0.61 | 0.9351 | 10.3 | 94.2 | |
14 | AP (N10-C2) | 0.34 | 0.9256 | 5.55 | 78.4 | |
15 | AP (N10-C5) | 0.45 | 0.9351 | 7.45 | 87.6 | |
16 | AP (N10-C10) | 0.57 | 0.9782 | 9.45 | 93.0 | |
17 | AP (N10-C20) | 0.64 | 0.936 | 10.7 | 95.0 | |
18 | AP (N20-C10) | 0.54 | 0.9769 | 9.00 | 91.6 | |
B. Effect of operation variables on the AP (N10-C10) photocatalytic performance | ||||||
Order | Parameter | Decay rate (min-1) | R2 | CADR (L min-1) | RE (%) | |
(1) FA concentration (ppm) | ||||||
19 | 0.5 | 1.14 | 0.9795 | 19.1 | 100 | |
20 | 1 | 0.80 | 0.9792 | 13.5 | 98.0 | |
21 | 3 | 0.67 | 0.9666 | 11.2 | 95.3 | |
22 | 5 | 0.57 | 0.9782 | 9.45 | 93.0 | |
(2) AP flow rate (L min-1) | ||||||
23 | 100 | 0.52 | 0.9943 | 8.73 | 92.0 | |
24 | 130 | 0.54 | 0.9901 | 9.07 | 92.6 | |
25 | 160 | 0.57 | 0.9782 | 9.45 | 93.0 | |
(3) Gas humidity (RH, %) | ||||||
26 | 0 | 0.57 | 0.9782 | 9.45 | 93.0 | |
27 | 20 | 0.31 | 0.9967 | 5.10 | 79.0 | |
28 | 50 | 0.21 | 0.9948 | 3.33 | 64.6 | |
29 | 100 | 0.14 | 0.983 | 2.24 | 49.6 |
Fig. 7. The effects of process variables on the performance of AP (N10-C10) honeycomb filter. (a) FA concentration (0.5-5 ppm); (b) AP flow rate (100-160 L min-1); and (c) RH (0-100%).
Order | Photocatalyst | Light source | Mass of catalyst (mg) | Concentration (ppm) | Irradiation time (h) | Chamber volume (L) | Humidity (%) | Flow rate (L min-1) | Conversion (%) | ke (min-1) | CADR (L min-1) | n-CADR (L min-1 g-1) | Quantum yield (molecules photon-1) | Space-time yield (molecules photon-1 mg-1) | Ref. |
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
1 | TiO2/rGO | 30 W UV lamp | 200 | 1.00 | 6.00 | 216 | aNA | NA | 92.0 | 0.008 | 1.69* | 8.44* | 4.11.E-06 | 2.06.E-08 | [ |
2 | C3N4/TiO2 | 15 W UV lamp | 300 | 170 | 1.00 | 15.0 | NA | NA | 94.0 | 0.064 | 0.95* | 3.18* | 5.95.E-04 | 1.98.E-06 | [ |
3 | TiO2/sepiolite | 20 W UV lamp | 10000 | 6.68 | 12.0 | 500 | 45 | NA | 88.0 | 0.002 | 1.17* | 0.12* | 4.56.E-05 | 4.56.E-09 | [ |
4 | K/C3N4 | 420 W Xenon lamp | 100 | 300 | 0.53 | 6.00 | 51 | NA | 97.7 | 0.093 | 0.56* | 5.57* | 3.05.E-05 | 3.05.E-07 | [ |
5 | Ag/F/N/W-TiO2 | 25 W Blue light UV LED | 2000 | 4.00 | 2.00 | 216 | NA | NA | 88.1 | 0.018 | 3.96* | 1.98* | 4.71.E-05 | 2.35.E-08 | [ |
6 | AP (Pt@Cu/TiO2) | 1 W Air purifier UV-LED | 50 | 0.5 | 0.17 | 17.0 | < 1 | 160 | 100 | 0.925 | 15.9 | 318 | 1.94.E-04 | 3.88.E-06 | [ |
7 | AP (N10-C10) | 1 W Air purifier UV-LED | 59.9 | 5.00 | 0.08 | 17.0 | < 1 | 160 | 93.0 | 0.565 | 9.45 | 158 | 3.49.E-03 | 5.82.E-05 | This study |
Table 4 Comparison of the photocatalytic performance metrics of N-TiO2 photocatalysts (i.e., AP (N10-C10)) in this work with others reported previously.
Order | Photocatalyst | Light source | Mass of catalyst (mg) | Concentration (ppm) | Irradiation time (h) | Chamber volume (L) | Humidity (%) | Flow rate (L min-1) | Conversion (%) | ke (min-1) | CADR (L min-1) | n-CADR (L min-1 g-1) | Quantum yield (molecules photon-1) | Space-time yield (molecules photon-1 mg-1) | Ref. |
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
1 | TiO2/rGO | 30 W UV lamp | 200 | 1.00 | 6.00 | 216 | aNA | NA | 92.0 | 0.008 | 1.69* | 8.44* | 4.11.E-06 | 2.06.E-08 | [ |
2 | C3N4/TiO2 | 15 W UV lamp | 300 | 170 | 1.00 | 15.0 | NA | NA | 94.0 | 0.064 | 0.95* | 3.18* | 5.95.E-04 | 1.98.E-06 | [ |
3 | TiO2/sepiolite | 20 W UV lamp | 10000 | 6.68 | 12.0 | 500 | 45 | NA | 88.0 | 0.002 | 1.17* | 0.12* | 4.56.E-05 | 4.56.E-09 | [ |
4 | K/C3N4 | 420 W Xenon lamp | 100 | 300 | 0.53 | 6.00 | 51 | NA | 97.7 | 0.093 | 0.56* | 5.57* | 3.05.E-05 | 3.05.E-07 | [ |
5 | Ag/F/N/W-TiO2 | 25 W Blue light UV LED | 2000 | 4.00 | 2.00 | 216 | NA | NA | 88.1 | 0.018 | 3.96* | 1.98* | 4.71.E-05 | 2.35.E-08 | [ |
6 | AP (Pt@Cu/TiO2) | 1 W Air purifier UV-LED | 50 | 0.5 | 0.17 | 17.0 | < 1 | 160 | 100 | 0.925 | 15.9 | 318 | 1.94.E-04 | 3.88.E-06 | [ |
7 | AP (N10-C10) | 1 W Air purifier UV-LED | 59.9 | 5.00 | 0.08 | 17.0 | < 1 | 160 | 93.0 | 0.565 | 9.45 | 158 | 3.49.E-03 | 5.82.E-05 | This study |
Fig. 9. The comparison of the characteristics of AP (Nx-C10; x = 0 and 10) before and after photocatalytic oxidation of FA. (a,b) Raman spectra; (c) XRD; (d) FTIR.
Fig. 11. The photocatalytic reaction of FA over AP (N10-C10). (a) Schematic for the photocatalytic mineralization pathway; (b) FA conversion efficiency (%) to CO2.
Fig. 12. Identified ROSs generated in the reaction mechanism. EPR signals of the DMPO-?OH (a) and DMPO-?O2 (b) by AP (Nx-C10) filters; (c) Gaseous scavenger test for ?1O2, ?O2-, and ?OH radicals during the photocatalytic degradation of FA (100 ppm) onto AP (N10-C10) filter under UV irradiation.
Fig. 13. Partial densities for chemically active Ti-atom on {101} surface of TiO2 without (a) and with (b) oxygen vacancies, without N-impurity (solid black line), with N-impurity before (solid red line) and after (dashed blue line) first step of conversion of FA molecules.
Fig. 14. Optimized atomic structures of the most energetically favorable steps of conversion FA and oxygen to CO2 and water on nitrogen-doped {110} and the surface of anatase TiO2 without oxygen vacancies (a-e) and {101} surface of anatase TiO2 with oxygen vacancy near nitrogen center (f-j). Panels (a) and (f) show the physical adsorption of FA and oxygen molecules near nitrogen defects. Panels (b-d) and (g-f) demonstrate intermediate steps corresponding with covalent attachment of the reactants and products to Ti3+ sites near nitrogen defects. Panels (e) and (j) show the final products of the reaction (carbon monoxide and water) non-covalently attached to catalytic surfaces.
Order | Reaction steps | Substrate (ΔH: kJ mol-1) | ||
---|---|---|---|---|
{110}+NO | {101}+NO | {101}+NO+OVs | ||
1 | FA + O2 adsorption | -79.6 | -69.2 | -78.1 |
2 | water adsorption | -74.9 | 116.6 | 121.2 |
3 | H2CO + O2 → *-OCH + *-OOH | 103.7 | -173.7 | -186.3 |
4 | *-CHO + *-OOH → *-CHOOH + *-O | -253.9 | -567.7 | -538.1 |
5 | *-CHOOH + *-O → *-COOH +*-OH | -519.1 | 79.2 | -95.3 |
6 | *-COOH +*-OH → CO2 + H2O | 98.3 | -192.8 | -53.5 |
7 | CO2 + H2O desorption | 150.8 | 108.6 | 114.1 |
Table 5 Calculated enthalpies (ΔH: kJ/mol) for the conversion reactions of FA to CO2 over {110} and {101} surfaces of anatase TiO2 with substitutional nitrogen impurity (No) and oxygen vacancies (OVs). An asterisk denotes the substrate.
Order | Reaction steps | Substrate (ΔH: kJ mol-1) | ||
---|---|---|---|---|
{110}+NO | {101}+NO | {101}+NO+OVs | ||
1 | FA + O2 adsorption | -79.6 | -69.2 | -78.1 |
2 | water adsorption | -74.9 | 116.6 | 121.2 |
3 | H2CO + O2 → *-OCH + *-OOH | 103.7 | -173.7 | -186.3 |
4 | *-CHO + *-OOH → *-CHOOH + *-O | -253.9 | -567.7 | -538.1 |
5 | *-CHOOH + *-O → *-COOH +*-OH | -519.1 | 79.2 | -95.3 |
6 | *-COOH +*-OH → CO2 + H2O | 98.3 | -192.8 | -53.5 |
7 | CO2 + H2O desorption | 150.8 | 108.6 | 114.1 |
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