氮掺杂对环境空气中TiO2纳米催化剂抗甲醛光催化矿化的影响

doi:10.1016/S1872-2067(24)60010-0

催化学报 ›› 2024, Vol. 59: 303-323.DOI: 10.1016/S1872-2067(24)60010-0

氮掺杂对环境空气中TiO₂纳米催化剂抗甲醛光催化矿化的影响

Dae-Hwan Lim^a, Aadil Bathla^a, Hassan Anwer^b, Sherif A. Younis^a^,^c, Danil W. Boukhvalov^d^,^e, Ki-Hyun Kim^a^,^*()

^a汉阳大学土木与环境工程系, 首尔, 韩国
^b国立科技大学环境工程系, 伊斯兰堡, 巴基斯坦
^c埃及石油研究所分析与评估部, 开罗, 埃及
^d南京林业大学材料物理与化学研究所, 理学院, 江苏南京, 中国
^e乌拉尔联邦大学物理与技术研究所, 叶卡捷琳堡, 俄罗斯

收稿日期:2024-01-16 接受日期:2024-02-14 出版日期:2024-04-18 发布日期:2024-04-15
通讯作者: *电子信箱: kkim61@hanyang.ac.kr (K.-H. Kim).

The effects of nitrogen-doping on photocatalytic mineralization of TiO₂ nanocatalyst against formaldehyde in ambient air

Dae-Hwan Lim^a, Aadil Bathla^a, Hassan Anwer^b, Sherif A. Younis^a^,^c, Danil W. Boukhvalov^d^,^e, Ki-Hyun Kim^a^,^*()

^aDepartment of Civil and Environmental Engineering, Hanyang University, 222 Wangsimni-ro, Seongdong-Gu, Seoul 04763, Korea
^bDepartment of Environmental Engineering, National University of Sciences and Technology, H-12, Islamabad 44000, Pakistan
^cAnalysis and Evaluation Department, Egyptian Petroleum Research Institute, Nasr City, Cairo 11727, Egypt
^dCollege of Science, Institute of Materials Physics and Chemistry, Nanjing Forestry University, Nanjing 210037, Jiangsu, China
^eInstitute of Physics and Technology, Ural Federal University, Yekaterinburg 620002, Russia

Received:2024-01-16 Accepted:2024-02-14 Online:2024-04-18 Published:2024-04-15
Contact: *E-mail: kkim61@hanyang.ac.kr (K.-H. Kim).

摘要/Abstract

摘要：

通过氮掺杂TiO₂(N-TiO₂)浸渍蜂窝过滤器构建了一系列原型光催化空气净化器(AP(N_x-C_y))系统, 并用于在UV-LED光(1 W)照射条件下光催化分解0.5-5 ppm甲醛(CH₂O)蒸汽. 在上述催化过滤器系统中, N_x和C_y分别代表N/Ti摩尔比(0-20)和N-TiO₂浓度(2-20 mg mL^-1). 光催化分解实验结果表明, AP(N₁₀-C₁₀)的性能最好, 其催化CH₂O转化为CO₂的转化率最高, 循环反应10次后CO₂产率仍达到89.2%, 在干燥空气中的清洁空气输送速率为9.45 L min^-1. N₁₀-C₁₀的电荷载流子寿命(τ_a: 1.70 ns)优于其他样品(如纯TiO₂的电荷载流子寿命为1.37 ns), 这表明N缺陷(N_o)有助于降低带隙(3.10 eV)和产生氧空位OVs-Ti³⁺, 这与密度泛函理论(DFT)模拟结果一致.

采用原位漫反射红外傅里叶变换、电子顺磁共振和DFT分析等多种方法研究了CH₂O的光催化氧化途径. 结果表明, 氧化过程涉及多个能量有利的中间步骤(例如CH₂O以CH₂O₂的形式在TiO₂-OV {110} 表面的桥连O/OH基团上发生放热共价吸附, 随后通过催化脱氢/氧化反应直接生成CO₂: CH₂O₂/HCOO^- + •OH → H₂O + CO₂）. 这些步骤与具有N杂质的{101}表面上化学活性Ti原子的态密度计算结果一致. 预计N_o缺陷和OVs的存在将通过降低活化能垒来影响反应能量和中间产物, 从而在加湿条件下实现有效的矿化.

综上, 本文为设计和构建先进的光催化系统, 并用于环境空气中醛类挥发性有机物(VOCs)的有效矿化提供了新思路.

关键词: 光催化蜂窝过滤器, 甲醛, 氮掺杂TiO₂, 密度泛函理论计算, 催化反应途径, 空气净化

Abstract:

A series of proto-type photocatalytic air purifier (AP (N_x-C_y)) systems are built with a nitrogen-doped TiO₂ (N-TiO₂)-impregnated honeycomb (HC) filter for photocatalytic decomposition of 0.5-5 ppm formaldehyde (FA: CH₂O) vapor under varying conditions and UV-LED light (1 watt). The binary codes of N_x and C_y in AP systems are used as the composition identifiers to represent N/Ti molar ratios (0 to 20) and N-TiO₂ concentration (2 to 20 mg mL^-1), respectively. The AP (N₁₀-C₁₀) is found as an optimum unit with the highest capability to boost the catalytic conversion of CH₂O to CO₂ (yield = 89.2% over 10^th cycles and the clean air delivery rate (CADR) of 9.45 L min^-1 in dry air). The superior charge carrier lifetime (τ_a: 1.70 ns) of N₁₀-C₁₀ over others (e.g., 1.37 ns for pure TiO₂) should indicate the influential role of N-defects (N_o) in reducing the bandgap (3.10 eV) and in creating defect-related oxygen vacancy (OVs-Ti³⁺) states as predicted by the density functional theory (DFT) simulation. The photocatalytic oxidation pathway of CH₂O, when assessed by diverse approaches (e.g., in-situ diffuse reflectance infrared Fourier transform, electron paramagnetic resonance, and DFT analyses), is found to involve several energetically favorable intermediate steps (such as exothermic covalent adsorption of CH₂O to bridged O/OH groups on TiO₂-OV {110} surface in the form of CH₂O₂ followed by catalytic dehydrogenation/oxidation reactions to yield CO₂ through direct route: CH₂O₂/HCOO^- + •OH → H₂O + CO₂). These steps are supported by the calculated density of states (DOS) for chemically active Ti-atom on {101} surface with N-impurity. The presence of N_o-defects and OVs is expected to influence the reaction energetics and intermediates for efficient mineralization in humidified conditions by lowering the activation barriers. This study offers valuable insights into the design and construction of an advanced photocatalytic system for efficient mineralization of aldehyde VOCs in ambient air.

Key words: Photocatalytic honeycomb filter, Formaldehyde, Nitrogen-doped TiO₂, Density functional theory calculations, Catalysis reaction pathways, Air purification

Dae-Hwan Lim, Aadil Bathla, Hassan Anwer, Sherif A. Younis, Danil W. Boukhvalov, Ki-Hyun Kim. 氮掺杂对环境空气中TiO₂纳米催化剂抗甲醛光催化矿化的影响[J]. 催化学报, 2024, 59: 303-323.

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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https://www.cjcatal.com/CN/Y2024/V59/I4/303

图/表 19

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

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 (S_BET, m² g^-1)	Pore volume (V_t, cm³ g^-1)	Average pore diameter (d_p, 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. 2. Morphological characterization using TEM. (a) AP (N0-C10); (b) AP (N1-C10); (c) AP (N5-C10); (d) AP (N10-C10).

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. 5. Electrochemical analysis of AP (Nx-C10; x =0, 1, 5, 10, and 20) filters. (a) Transient photocurrent; (b) EIS 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).

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%).

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 (%)	k_e (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	[97]
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	[98]
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	[99]
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	[100]
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	[101]
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	[87]
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. 8. Reusability of AP (N10-C10) photocatalytic filters against FA (5 ppm) degradation over ten reuse cycles.

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. 10. The in-situ DRIFT of AP (N10-C10) under UV Off (FA + O2), UV On (FA + O2), and UV On (FA + O2 + H2O) conditions.

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.

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)
Order	Reaction steps	{110}+N_O	{101}+N_O	{101}+N_O+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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氮掺杂对环境空气中TiO₂纳米催化剂抗甲醛光催化矿化的影响

The effects of nitrogen-doping on photocatalytic mineralization of TiO₂ nanocatalyst against formaldehyde in ambient air

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