Lead-Free Halide Perovskite Nanocrystals: A New Generation of Photocatalytic Materials

Qianqian Fan; Lu Wen; Jianzhong Ma

doi:10.7536/PC210922

Progress in Chemistry ›› 2022, Vol. 34 ›› Issue (8) : 1809-1814 DOI: 10.7536/PC210922

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Lead-Free Halide Perovskite Nanocrystals: A New Generation of Photocatalytic Materials

Qianqian Fan ¹^,²^,³^,^*
, Lu Wen ²^,³
, Jianzhong Ma ¹^,²^,³^,^*

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Abstract

TiO₂ based photocatalytic technology is of wide application in the fields of pollutant degradation, CO₂ reduction, hydrogen production, etc. owing to its set of intriguing properties, including fast reaction speed, high visible light utilization efficiency, and no secondary pollution. However, the low utilization rate of visible light for TiO₂ materials limits it further use. In recent years, lead-free halide perovskite nanocrystals are of great interest in the field of photocatalysis due to their notable advantages such as tunable band gap and high visible light absorption. Relevant studies show that lead-free halide perovskite nanocrystals can be successfully applied in the fields of CO₂ reduction and organic pollutant degradation, with significant effects. This review describes the preparation methods of lead-free halide perovskite nanocrystals, and summarizes its applications in the fields of CO₂ reduction, hydrogen production, pollutant degradation and NO removal systematically. Finally, the current issues of lead-free halide perovskite nanocrystals as photocatalytic materials and the outlook for the future directions are discussed and prospected.

Contents

1 Introduction

2 Preparation methods of lead-free halide perovskite nanocrystal

2.1 Ligand-assisted reprecipitation

2.2 Heat injection

2.3 Other methods

3 Application of lead-free halide perovskite nanocrystals in the field of photocatalysis

3.1 CO₂reduction

3.2 Hydrogen production

3.3 Degradation of organic pollutants

3.4 NO removal

4 Conclusion and outlook

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Keywords

lead-free halide perovskite nanocrystals / new photocatalytic materials / CO₂reduction / hydrogen production / degradation of pollutants

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Qianqian Fan, Lu Wen, Jianzhong Ma. Lead-Free Halide Perovskite Nanocrystals: A New Generation of Photocatalytic Materials. Progress in Chemistry, 2022, 34(8): 1809-1814 DOI:10.7536/PC210922

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1 Preface

In 1972, Fujishima and Honda reported the research on hydrogen production by photocatalytic decomposition of H₂O using TiO₂ single crystal in Nature, which opened the era of TiO₂ photocatalytic materials^[1]. With the further development of photocatalytic technology, more and more materials have been successfully used in the field of photocatalysis. At present, the reported photocatalytic materials include oxide perovskite, metal oxide, sulfide, nitride, phosphide and so on^[2⇓⇓~5]^[6⇓~8]^[9]^[10]^[11]. However, traditional photocatalytic materials are generally faced with the problems of narrow light absorption range, low utilization of visible light, complex preparation process and low photocatalytic efficiency^[12⇓~14]. Therefore, it is urgent to develop a new generation of photocatalytic materials.

In recent years, lead-based halide perovskite nanocrystals (chemical composition of APbX₃, where A=CH₃NH₃, CH(NH₂)₂, or Cs, etc., and X = Cl, Br, or I) have strong light absorption ability, high carrier mobility, and tunable band gap, which make them ideal photocatalytic materials and have been successfully used in the fields of photocatalytic hydrogen production, CO₂ reduction, and dye degradation with remarkable effects^[15,16]^[17]. However, this kind of perovskite materials contains lead element which is harmful to human body and environment, limiting its wide application. In this situation, lead-free halide perovskite nanocrystals, which can not only avoid the use of toxic metal elements, but also retain the excellent characteristics of perovskite, emerge as the times require. Lead-free halide perovskite nanocrystals are usually obtained by replacing Pb²⁺ in APbX₃ with non-toxic or low-toxic metal ions (such as Sn, Sb, Bi, Ag, etc.), which have low toxicity and similar structure to lead-based halide perovskites, and have rapidly become a research hotspot in the field of photocatalysis. In 2018, Zhou et al. Successfully achieved CO₂ reduction with Cs₂AgBiBr₆ nanocrystals as catalyst for the first time^[18]. After that, Bresolin et al. And Zhang et al. Respectively verified that (CH₃NH₃)₃Bi₂I₉ and Cs₂AgBiBr₆ could be used as visible-light-responsive photocatalysts for the degradation of environmental pollutants^[19,20]. Up to now, lead-free halogen perovskite nanocrystals have been successfully applied in the fields of photocatalytic hydrogen production, CO₂ reduction and pollutant degradation.

In the previous research, our research group carried out a series of studies on the preparation and performance improvement of lead-free halogen perovskite nanocrystals, and successfully applied them to the photocatalytic degradation of pollutants^[21,22]. Based on the previous work and extensive literature research, this paper mainly reviews the research progress of lead-free halide perovskite nanocrystals as a new generation of photocatalysts, focusing on the preparation of lead-free halide perovskite nanocrystals and their application in the field of photocatalysis. Finally, the existing problems and future research directions of lead-free halide perovskite nanocrystals in the field of photocatalysis were prospected.

2 Method for preparing lead-free halogen system perovskite nanocrystalline

2.1 Ligand-assisted recrystallization

ligand-assisted reprecipitation (LARP) is one of the most common methods for the preparation of halogen perovskite nanocrystals, which has the advantages of mild conditions, simple operation and high yield. The LARP method is to dissolve the perovskite precursor and organic ligand in its good solvent, and then disperse them in the anti-solvent of the precursor, so that the precursor in the system reaches a supersaturated state in a short time, and spontaneous precipitation and crystallization occur to form nanocrystals^[23,24]. Leng et al. Reported a study on the preparation of MA₃Bi₂Br₉ nanocrystals by the LARP method using N, N-dimethylformamide (DMF) and ethyl acetate (EAC) as good solvents for MABr and BiBr₃, and Octane as an anti-solvent, and the specific synthesis process is shown in Fig. 1^[25]. It was found that the introduction of organic ligand n-octylamine (OLAm) could control the crystallization rate of the crystal, while the introduction of oleic acid (OA) was beneficial to stabilize the nanocrystal solution. Yang et al. First synthesized Cs₃Bi₂Br₉ nanocrystals by the LARP method, using dimethyl sulfoxide (DMSO) as a good solvent for CsBr and BiBr₃, isopropanol as an anti-solvent, and OA as a ligand^[26]. It was found that the photoluminescence quantum efficiency (PLQE) increased from 0. 2% to 4% when the amount of OA was 5%.

2.2 Hot injection method

Compared with the LARP method, the particle size distribution of perovskite nanocrystals prepared by the hot injection method is more uniform, so it is widely used in the preparation of lead-free perovskite nanocrystals. The hot injection method is usually to rapidly inject the precursor solution into another hot solution containing ligands at a high temperature above 120 ℃, and then the crystal nucleates and gradually forms perovskite nanocrystals, and the crystal size can be effectively adjusted by controlling the injection temperature, reaction time and precursor concentration^[23,24].

Jellicoe et al. Dissolved SnX₂(X=I/Br/Cl) in tri-n-octylphosphine at high temperature to form a Sn-containing precursor solution (Sn-precursor), and then injected the precursor solution into a mixed solution containing Cs₂CO₃, OA, oleylamine (OLA) and 1-octadecene (ODE) at 170 ° C, and after a certain reaction time, the CsSnX₃(X=I/Br/Cl) nanocrystals were obtained, and the preparation schematic diagram is shown in Fig. 2^[27]. The results show that the band gap of CsSnX₃ nanocrystals can be effectively controlled (from 2. 8 eV to 1. 3 eV) based on the quantum confinement effect and the change of halide composition in perovskite crystals. Pal et al. Prepared Sb-containing precursor by heating and mixing Sb₂O₃ with caprylic acid and organic amine, and then injected cesium oleate precursor solution into the Sb precursor solution to obtain Cs₃Sb₂I₉ nanocrystals^[28]. The results show that the morphology of Cs₃Sb₂I₉ nanocrystals can evolve from nanosheets (at 180 ℃) to nanorods (at 220 ℃) by changing the reaction temperature, and this method can also be used to prepare Rb₃Sb₂I₉ nanocrystals.

2.3 Other methods

In addition to LARP and thermal injection methods, ultrasonic method, solid state synthesis method and hydrothermal method have also been used to prepare lead-free perovskite nanocrystals. Bhosale et al. Prepared A₃Bi₂I₉(A=Rb, Cs, CH₃NH₃) nanocrystals by ultrasonic method, adding BiI₃ and AI (A = Rb, Cs, CH₃NH₃) into DMF,A₃Bi₂I₉(A=Rb, Cs, CH₃NH₃) perovskite nanocrystals were obtained by grinding in a glove box with the addition of OA and OLA and sonication for 3 – 5 d^[29]. Cao et al. Obtained Cs₂NaVCl₃ nanocrystals by conventional solid phase synthesis method by uniformly grinding and placing the mixture of CsCl, NaCl and VCl₃ in a quartz tube, sealing and heating in a muffle furnace^[30]. Solid phase synthesis has the advantages of high selectivity, high yield and simple process. At the same time, they also successfully prepared Cs₂NaVCl₃ nanocrystals by hydrothermal method, that is, adding V₂O₃ and HCl solution into a high-pressure reactor, sealing and heating to 150 ° C, adding CsCl and NaCl after 2 H of reaction, and continuing to heat at 150 ° C for 2 H to obtain Cs₂NaVCl₃ nanocrystals. The schematic diagram of the specific hydrothermal reaction process is shown in Figure 3.

3 Application of Lead-free Halogen Perovskite Nanocrystals in Photocatalysis

3.1 Field of CO₂ reduction

Photocatalytic reduction of CO₂ using semiconductor materials to synthesize combustible materials is an ideal way to solve the energy crisis and alleviate the greenhouse effect. Lu et al. Prepared Cs₃Sb₂Br₉ nanocrystals with uniform size by hot injection method^[31]. It was found that the photocatalytic reduction of CO₂ by Cs₃Sb₂Br₉ nanocrystals could obtain a single product of CO, and compared with CsPbBr₃ nanocrystals, the photocatalytic efficiency was improved by 10 times within 4 H, reaching 510μmol·g^-1h^-1. Zhou et al. Studied the performance of Cs₂AgBiBr₆ nanocrystals for photocatalytic reduction of CO₂^[18]. The results show that the Cs₂AgBiBr₆ nanocrystals have good light, thermal and moisture stability, and the CO₂ can be reduced to CO and CH₄ under visible light irradiation for 6 H, and the yields are 14.1μmol·g^-1 and 9.6μmol·g^-1, respectively. In order to improve the photocatalytic rate and the stability of recycling, it is very important to construct a surface heterojunction with a coating structure by interface engineering to promote the separation and migration efficiency of photogenerated carriers in lead-free halide perovskite nanocrystals. Wang et al. Constructed Cs₂AgBiBr₆@g-C₃N₄Z type heterojunction structure and Cs₂AgBiBr₆@g-C₃N₄Ⅱ type heterojunction structure in toluene and CH₂Cl₂, respectively^[32]. The results show that the existence of the Cs₂AgBiBr₆@g-C₃N₄,Z type heterojunction structure with a type II heterojunction structure enables the Cs₂AgBiBr₆@g-C₃N₄ to show excellent CH₄ yield performance in photocatalytic CO₂ reduction,The yield was 10 and 16 times higher than that of pure g-C₃N₄ and pure Cs₂AgBiBr₆, respectively. In the cycle stability test, the decomposition of Cs₂AgBiBr₆ began to occur after 5 H of reaction cycle, and the photocatalytic efficiency decreased significantly, while the photocatalytic performance of Cs₂AgBiBr₆@g-C₃N₄ for the reduction of CO₂ was almost unchanged after 12 H of recycling, which proved that the construction of the above core-shell coating structure was an effective way to improve the stability of lead-free halide perovskite catalysts^[20].

3.2 Field of hydrogen production

Hydrogen, known as green energy, can be obtained from water or hydrohalic acid by photocatalysis, which is one of the key ways to alleviate the shortage of petrochemical resources. Guo et al. Prepared lead-free perovskite (CH₃NH₃)₃Bi₂I₉ nanocrystals by hydrothermal method, which showed excellent photocatalytic cycling stability under visible light irradiation^[33]. At the same time, when (CH₃NH₃)₃Bi₂I₉ nanocrystals were used as the main catalyst and platinum was used as the co-catalyst, the photocatalytic yield of H₂ could reach 169.21μmol·g^-1h^-1, which was 14 times higher. Wang et al. Found that the composite of Cs₂AgBiBr₆ nanocrystals and reduced graphene oxide (r-GO) could also be used for H₂ precipitation in saturated HBr aqueous solution, and the introduction of r-GO was beneficial to the separation and transfer of charges in Cs₂AgBiBr₆ nanocrystals^[34]. The Cs₂AgBiBr₆/r-GO composite exhibited a H₂ yield of 489μmol·g^-1 under visible light irradiation for 10 H and could exhibit high stability within 120 H. Malavasi et al. Reported DMASnBr₃ perovskite nanocrystals with excellent water resistance, which were compounded with g-C₃N₄ for photocatalytic hydrogen production^[35]. It is found that under the irradiation of simulated sunlight, the hydrogen evolution rate in the aqueous solution of DMASnBr₃@g-C₃N₄ can reach 1700μmol·g^-1·h^-1, and the effect is remarkable.

3.3 Field of organic pollutant degradation

It has been one of the challenging tasks in the field of ecological environment to efficiently and safely eliminate organic pollutants with low concentration, high toxicity and difficult degradation. Photocatalysis can effectively degrade, decolorize and detoxify organic pollutants, so that they can be degraded into inorganic small molecules such as CO₂ and H₂O, thus reducing the harm to the environment. Li et al. Used Cs₂AgInCl₆ nanocrystals to photocatalytically degrade Sudan red dye, and found that about 98.5% of Sudan red 3 could be degraded in 16 min under ultraviolet irradiation, and it still had good photocatalytic activity after five cycles^[36]. In addition, the Cs₂AgInCl₆ nanocrystals can also be used for the efficient degradation of rhodamine B, methyl orange and methyl red, and show efficient and stable photocatalytic degradation performance in ethanol solvent. Zhang et al. Prepared a MASnI₃/TiO₂(MA=CH₃NH₃⁺) composite photocatalyst with a heterojunction structure^[37]. The results show that when the composite ratio of MASnI₃ and TiO₂ is 1 ∶ 9, MASnI₃/TiO₂ can degrade 97% of rhodamine B in 40 min, showing a higher photocatalytic degradation ability than MASnI₃ nanocrystals and TiO₂.

3.4 Field of NO removal

Nitric oxide (NO) mainly comes from the consumption of fossil energy, and its emission can cause a series of environmental problems, such as acid rain, haze and photochemical smog, which seriously endanger human health^[38]. Acid absorption and alkali absorption are the commonly used methods to remove NO, but their costs are high^[39]. The removal of NO by photocatalytic technology to convert it into NO₂ is a relatively green and environmentally friendly method at present, so it has attracted much attention. Huo et al. Used aminated silica spheres loaded with FAPbBr₃ nanocrystals as a catalyst to remove NO, and found that the FAPbBr₃ nanocrystals had a high NO removal efficiency and the catalytic activity of the composite material was relatively stable in the photocatalytic process, but the potential harm of lead-containing perovskite to the environment limited its large-scale application^[40]. Based on this, Wu et al. Synthesized lead-free Cs₂AgBiBr₆ double perovskite nanocrystals by hot injection method, which can remove 97% NO in 30 min under visible light irradiation, and the removal rate of NO is nearly three times higher than that of lead-containing halogen-based CsPbBr₃ nanocrystals, and it shows excellent stability in four cycles, so it has great application prospects^[41]^[42].

To sum up, lead-free perovskite nanocrystals have attracted much attention due to their high carrier mobility, tunable band gap and strong optical absorption. However, some of the reported lead-free perovskite materials have large optical band gaps, such as Cs₂AgInCl₆(3.33 eV), DMASnBr₃(2.85 eV) and MAGeCl₃(3.76eV), which can only be used for photocatalytic reactions under UV excitation. In practical applications, lead-free perovskite nanocrystals with corresponding band gaps can be selected for photocatalysis according to the type of light source in the application environment. Among them, perovskite nanocrystals with small band gap are convenient for practical application because of their good photocatalytic performance under visible light. Therefore, the band gap width of lead-free perovskite can be adjusted by controlling the metal cations at the A-site, halogen elements at the X-site or doping in the follow-up study, so as to expand its application range.

The photocatalytic performance and application effect of lead-free halide perovskite nanocrystals are different when their components are different. In order to facilitate comparative analysis, the photocatalytic performance and application fields of several common lead-free halide perovskite nanocrystals are summarized, as shown in Table 1.

4 Conclusion and prospect

At present, lead-free halide perovskite nanocrystals as photocatalytic materials have been successfully applied in many fields, such as CO₂ reduction and pollutant degradation, showing obvious advantages, but the research in the field of photocatalysis is still at a preliminary stage, and its stability mechanism, carrier migration, recombination mechanism and photocatalytic mechanism still need to be further explored. As a new generation of photocatalytic materials, the existing problems and future development direction of lead-free halide perovskite nanocrystals at present are analyzed as follows:

(1) improving the stability of the lead-free halogen system perovskite nanocrystalline. First of all, lead-free halide perovskites are often difficult to exist stably in polar solvents due to their ionic structure characteristics, which limits their application in the field of photocatalysis to a certain extent, especially in water pollution treatment. Conventional stability improvement methods, such as organic ligand or inorganic material coating, can improve its stability, but reduce its light absorption rate, affecting the rapid migration of charge carriers in the photocatalytic process. In the later research, semiconductor photocatalytic materials can be used to compound with perovskite or coated with organic ligands which are conducive to carrier migration, so as to improve the stability of perovskite and avoid its impact on photocatalytic performance.

(2) To explore the correlation between the metal components of lead-free perovskite nanocrystals and their photocatalytic properties. Different metal components in lead-free halogen perovskites (structural formula ABX₃, where B is a lead-free metal component replacing Pb, A=CH₃NH₃, CH(NH₂)₂ or Cs, etc., and X = Cl, Br or I) have great differences in crystal structure and band gap structure, and the final photocatalytic performance and application fields will also be different. In the future research, it is urgent to systematically explore the corresponding relationship between the metal component and its crystal structure and band gap structure, and to obtain the influence of the metal component on the photocatalytic performance of lead-free halide perovskite nanocrystals.

(3) Promote the industrialization process of lead-free halogen perovskite nanocrystals in the field of photocatalysis. At present, the application of lead-free halogen perovskite nanocrystals in many fields, such as CO₂ reduction, hydrogen production and pollutant degradation, is still in the laboratory stage and has not yet been industrialized. The follow-up research in this area should be closely combined with the practical application needs, and in the process of research, it is necessary to systematically investigate the recycling stability, cost and practical application efficiency of photocatalytic materials, so as to promote their industrialization process.

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Funding

National Natural Science Foundation of China (No. 52103088). Key Laboratory of Auxiliary Chemistry and Technology for Chemical Industry open fund(KFKT2020-08)

China Postdoctoral Science Foundation project(2020M683667XB)