Kinetic study of oxygen reduction reaction and PEM fuel cell performance of Pt/TiO2-C electrocatalyst

The electrochemical activity and thermal stability of the Pt/TiO₂-C were evaluated in the oxygen reduction reaction (ORR) in acid medium at different temperatures. The platinum was selectively deposited onto the TiO₂ (E_bg = 2.3 eV) by the photo-irradiation of platinum precursor (Pt⁴⁺→Pt⁰). The Pt/TiO₂-C electrocatalyst prepared was characterized by XRD, TEM/EDS, cyclic and lineal voltammetry techniques. TEM images indicated that platinum nanoparticles (<5 nm) were deposited in agglomerates form around the oxide sites. EDS and XRD results confirm the composition and crystalline structure of Pt/TiO₂-C. The thermal stability and electrochemical activity of the Pt/TiO₂-C for ORR at different temperatures (298–343 K) is higher than Pt/C commercial sample (Pt-Etek). A more favorable apparent enthalpy of activation for Pt/TiO₂-C was greatly influenced by addition of oxide in the catalyst compare to Pt-Etek. Single H₂/O₂ fuel cell performance results of Pt/TiO₂-C show an improvement of the power density with the increase of the temperature.     

Studies of electrochemical performance of carbon supported Pt-Cu nanoparticles as anode catalysts for direct borohydride-hydrogen peroxide fuel cell

Carbon supported Pt-Cu bimetallic nanoparticles are prepared by a modified NaBH₄ reduction method in aqueous solution and used as the anode electrocatalyst of direct borohydride-hydrogen peroxide fuel cell (DBHFC). The physical and electrochemical properties of the as-prepared electrocatalysts are investigated by transmission electron microscopy (TEM), X-ray diffraction (XRD), cyclic voltammetry (CV), chronoamperometry (CA), chronopotentiometry (CP) and fuel cell test. The results show that the carbon supported Pt-Cu bimetallic catalysts have much higher catalytic activity for the direct oxidation of BH₄⁻ than the carbon supported pure nanosized Pt catalyst, especially the Pt₅₀Cu₅₀/C catalyst presents the highest catalytic activity among all as-prepared catalysts, and the DBHFC using Pt₅₀Cu₅₀/C as anode electrocatalyst and Pt/C as cathode electrocatalyst shows as high as 71.6 mW cm⁻² power density at a discharge current density of 54.7 mA cm⁻² at 25 °C.     

Nitrogen doped carbon layer coated platinum electrocatalyst supported on carbon nanotubes with enhanced stability

Enhancement in durability of electrocatalyst is still one of the most important issues in polymer electrolyte fuel cells (PEFCs). Here, we report a structurally coated electrocatalyst supported on carbon nanotubes (CNT), in which platinum (Pt) nanoparticles are coated by nitrogen doped carbon (NC) layers. CNT/NC/Pt/NC shows comparable electrochemical surface area (ECSA) and oxygen reduction reaction (ORR) activity to the non-coated electrocatalyst (CNT/NC/Pt), indicating that NC layer on Pt nanoparticles almost negligibly affects the activities of electrocatalyst; while, CNT/NC/Pt/NC exhibits a higher Pt stability due to the unique structure, in which the Pt nanoparticles are stabilized by the NC layers and Pt aggregation is decelerated proved by TEM measurement. Maximum power density of CNT/NC/Pt/NC reached 604 mW cm^?2 with Pt loading of 0.1 mg_Pt cm^?2, which only decreases by 7% compared to CNT/NC/Pt (650 mW cm^?2). The electrochemical analysis and fuel cell test illustrate that NC layer on Pt nanoparticles enhances the durability without serious deterioration of fuel cell performance.     

Alcohol reduction-mediated preparation of a nano-scale Pt/C electrocatalyst for the oxygen reduction reaction in PEM fuel cells

A nano-scale Pt/C electrocatalyst for oxygen reduction in PEM fuel cells was prepared by alcohol-mediated reduction of the PtCl₆^2? ion complex on the carbon Vulcan XC-72. The effects of various parameters, including the types of precursor and reducing agent and their concentrations, the initial solution pH and the reaction time, were explored. The preliminary results indicated that the electrocatalyst prepared using ammonium hexachloroplatinate ((NH₄)₂PtCl₆) as the Pt²⁺ source provided a similar catalytic efficiency as that prepared from hexachloroplatinic acid (H₂PtCl₆). The nano-scale Pt/C electrocatalyst prepared using methanol (CH₃OH) as a reducing agent provided the smallest sized platinum particles with a uniform distribution in the nanometer range, a good particle dispersion and a high Pt content compared with that prepared using ethanol (C₂H₅OH) or 2-propanol (C₃H₇OH). The electrocatalyst prepared in an acidic solution yielded smaller sized platinum particles and a higher Pt content than that prepared in a basic solution. In addition, the concentration of the reducing agent and reaction time slightly affected both the Pt particle size and the Pt yield of the obtained electrocatalyst. Under apparent optimal conditions, the nano-scale Pt/C electrocatalyst had an electrochemical surface area of ～39.7 m²/g, which was ～1.9-fold higher than that of the commercial one. The performance of the electrocatalyst was also tested in a single PEM fuel cell in a H₂/O₂ atmosphere where compared to a commercial electrode a lower activation loss but higher ohmic loss was observed.     

Carbon paper supported Pt/Au catalysts prepared via Cu underpotential deposition-redox replacement and investigation of their electrocatalytic activity for methanol oxidation and oxygen reduction reactions

Through a simple and rapid method, carbon papers (CPs) were coated with Au and the resulting Au/CP substrates were used for the preparation of Pt/Au/CP by Cu underpotential deposition (Cu UPD) and redox replacement technique. A series of Pt_n/Au/CP catalysts (where n = number of UPD-redox replacement cycles) were synthesized and their electrochemical properties for methanol oxidation reaction (MOR), and oxygen reduction reaction (ORR) were investigated by electrochemical measurements. The Pt_n/Au/CP electrodes show higher electrocatalytic activity and enhanced poison tolerance for the MOR as compared to a commercial Pt/C on CP (Pt/C/CP). The highest mass specific activity and Pt utilization efficiency for MOR was observed on Pt₁/Au/CP with a thickness close to a monatomic Pt layer. Chronoamperometric tests in methanol solution revealed that Pt_n/Au/CPs have much higher CO tolerance compared to Pt/C/CP. Among the Pt_n/Au/CPs, CO tolerance decreases with increasing the amount of deposited Pt, indicating that the exposed Au atoms in close proximity to Pt plays a positive role against CO poisoning. Compared with the Pt/C/CP, all the Pt_n/Au/CP electrodes show more positive onset potentials and lower overpotentials for ORR. For instance, the onset potential of ORR is 150 mV more positive and the overpotential is ∼140 mV lower on Pt₄/Au/CP with respect to Pt/C/CP.     

ZIF derived mesoporous carbon frameworks with numerous edges and heteroatom-doped sites to anchor nano-Pt electrocatalyst

We report the use of nitrogen-doped three-dimensional carbon frameworks (N-MCF) to promote the catalytic performance of nano-sized Pt electrocatalyst for the catalysis of oxygen reduction reaction (ORR). The N-MCF, obtained by pyrolysis of zeolitic imidazolate framework, provides abundant edges, defects, and heteroatom-doped sites to anchor Pt nanoparticles, leading to strong Pt-support interaction and excellent particle dispersion within its three-dimensional mass transport channels. Electrochemical results show only 8 mV degradation in the half-wave potential after accelerated durability test for the N-MCF supported Pt catalysts. Meanwhile, the mass activity and specific activity of Pt/N-MFC could reach 246 mA mg⁻¹_Pt and 0.276 mA cm⁻² at 0.90 V_RHE, which is better than that of commercial Pt/C. Moreover, the high Pt utilization of Pt/N-MFC (186 mg _Pt kW⁻¹) could reach 1.9 times than that of fuel cell fabricated with commercial Pt/C cathode.     

PtRh alloys on hybrid TiO2 – Carbon support as high efficiency catalyst for ethanol oxidation

High cost and poor stability of catalysts remain major obstacles for the commercialization of direct ethanol fuel cells (DEFCs). In this work, a Pt₉Rh/TiO₂C nanostructured catalyst is synthesized via an impregnation-reduction method followed by thermal annealing in N₂ at ambient pressure. X-ray powder diffraction (XRD) and scanning transmission electron microscopy (STEM) are used to characterize the corresponding physico-chemical properties of the as-prepared catalysts. The results reveal that PtRh nanoparticles are uniformly distributed on the TiO₂C hybrid support material. Cyclic voltammetry, linear scan voltammetry, CO-stripping voltammograms, chronoamperometry and chronopotentiometry methods are employed to investigate their catalytic performance for ethanol oxidation. The results show that the Pt₉Rh/TiO₂C produced a current density of 1039.5 mA mg_Pt^?1, which are 3.98, 8.31 and 2.43 times higher than Pt/TiO₂C, Pt/C and Pt₉Rh/C, respectively. Furthermore, the Pt₉Rh/TiO₂C also has greater resistance to CO-poisoning and displays better stability for ethanol oxidation than other catalysts. Pt₉Rh/TiO₂C therefore provides a promising material for ethanol oxidation in direct ethanol fuel cells.     

Study of ethanol electro-oxidation in acid environment on Pt3Sn/C anode catalysts prepared by a modified polymeric precursor method under controlled synthesis conditions

A carbon-supported binary Pt₃Sn catalyst has been prepared using a modified polymeric precursor method under controlled synthesis conditions. This material was characterized using X-ray diffraction (XRD), and the results indicate that 23% (of a possible 25%) of Sn is alloyed with Pt, forming a dominant Pt₃Sn phase. Transmission electron microscopy (TEM) shows good dispersion of the electrocatalyst and small particle sizes (3.6 nm ± 1 nm). The polarization curves for a direct ethanol fuel cell using Pt₃Sn/C as the anode demonstrated improved performance compared to that of a PtSn/C E-TEK, especially in the intrinsic resistance-controlled and mass transfer regions. This behavior is probably associated with the Pt₃Sn phase. The maximum power density for the Pt₃Sn/C electrocatalyst (58 mW cm⁻²) is nearly twice that of a PtSn/C E-TEK electrocatalyst (33 mW cm⁻²). This behavior is attributed to the presence of a mixed Pt₉Sn and Pt₃Sn alloy phase in the commercial catalysts.     

Photodeposition of Pt nanoparticles onto TiO2@CNT as high-performance electrocatalyst for oxygen reduction reaction

The commonly used Pt/C catalyst has low durability for oxygen reduction reaction (ORR). In this work, CNT-supported TiO₂ nanoparticles, which synergistically combines the merits of TiO₂ (high stability and strong interactions with the supported Pt nanoparticles) and CNT (high specific surface area and large electrical conductivity), are prepared by a sol-gel process coupled with an annealing process and used as the support for Pt nanoparticles, which are anchored around TiO₂ nanoparticles by a photodeposition technique. The as-synthesized Pt/TiO₂@CNT catalyst exhibits a mass activity 5.3 times as large as that of the commercial Pt/C catalyst (0.358 A mg_Pt⁻¹ vs. 0.067 A mg_Pt⁻¹ at 0.9 V) and an excellent stability (no activity loss after 10000 potential cycles) for ORR, which can be mainly attributed to the lower oxygen adsorption energy of Pt, resulting from the strong metal-support interaction induced by the deposition of Pt nanoparticles around the well-dispersed TiO₂ nanoparticles on CNT.     

Emergent hierarchical porosity by ZIF-8/GO nanocomposite increases oxygen electroreduction activity of Pt nanoparticles

Hierarchically porous materials are promising as catalyst supports in fuel cells and batteries as they increase overall mass transfer and active site density. In this work, a hierarchically porous catalyst support for oxygen reduction reaction (ORR) in acidic media has been developed by a bottom-up approach. Graphene oxide (GO) was introduced during synthesis conditions of zeolitic imidazolate framework-8 (ZIF-8) to produce hybrid material of ZIF-8/GO. Successful nanocomposite formation was realized by preserved crystallinity and chemical interaction between species as revealed by X-ray diffraction and Fourier transform infrared spectroscopy. Introduction of GO and pyrolysis of resulting hybrid structure causes emergence of disordered meso/macropores with an accompanying increase in pore volume as revealed by N₂ sorption experiments. Pt nanoparticle deposition on pyrolyzed hybrid material by polyol method results in electrocatalyst Pt/NC-1, which shows greatly improved mass activity (182 vs 86 A g⁻¹_Pt) and specific activity (467 vs 186 μA g⁻¹_Pt) at 0.8 V for ORR against reference electrocatalyst Pt/r-GO and improved specific activity against Pt/C.     

PtCo incorporated porous carbon nanofiber as a promising oxygen reduction electrocatalyst

Designing oxygen reduction reaction (ORR) catalysts with high activity and long durability is significant for the development of proton exchange membrane fuel cells. Herein, the optimized platinum nanowires are used as templates for inducing growth of cobalt-containing metal-organic framework, deriving uniform nanofibers. After the calcination, the metal ions are transferred into the nitrogen-rich porous carbon, and wrapped by the carbon skeleton to form the PtCo bimetal incorporated nanofibers as high-performance ORR electrocatalyst. The Pt₄Co@NC-900 catalyst yields high specific activity (1.37 mA cm⁻²) in comparison to Pt/C (0.38 mA cm⁻²). The mass activity (MA) of Pt₄Co@NC-900 catalyst is approximately 3.8-fold higher than that of the commercial Pt/C under acidic conditions. After the accelerated durability tests, the Pt₄Co@NC-900 catalyst presents only 16% loss in MA, while Pt/C catalyst retains 73.0% of the initial MA. The improved ORR performance can be ascribed to the synergistic interaction between Co and Pt.     

Direct ethanol fuel cells based on PtSn anodes: the effect of Sn content on the fuel cell performance

In the present work, several carbon supported PtSn catalysts with different Pt/Sn atomic ratios were synthesized and characterized by X-ray diffraction (XRD), Transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). Both the results of TEM and XRD showed that all in-house prepared carbon supported Pt and PtSn catalysts had nanosized particles with narrow size distribution. According to the primary analysis of XPS results, it was confirmed that the main part of Pt of the as-prepared catalysts is in metallic state while the main part of Sn is in oxidized state. The performances of single direct ethanol fuel cells were different from each other with different anode catalysts and at different temperatures. It was found that, the single DEFC employing Pt₃Sn₂/C showed better performance at 60 °C while the direct ethanol fuel cells with Pt₂Sn₁/C and Pt₃Sn₂/C exhibited similar performances at 75 °C. Furthermore, at 90 °C, Pt₂Sn₁/C was identified as a more suitable anode catalyst for direct ethanol fuel cells in terms of the fuel cell maximum power density. Surface oxygen-containing species, lattice parameters and ohmic effects, which are related to the Sn content, are thought as the main factors influencing the catalyst activity and consequently the performance of single direct ethanol fuel cells.     

Performance of membrane electrode assemblies using PdPt alloy as anode catalysts in polymer electrolyte membrane fuel cell

Pd-based nanoparticles, such as 40 wt.% carbon-supported Pd₅₀Pt₅₀, Pd₇₅Pt₂₅, Pd₉₀Pt₁₀ and Pd₉₅Pt₅, for anode electrocatalyst on polymer electrolyte membrane fuel cells (PEMFCs) were synthesized by the borohydride reduction method. PdPt metal particles with a narrow size distribution were dispersed uniformly on a carbon support. The membrane electrode assembly (MEA) with Pd₉₅Pt₅/C as the anode catalyst exhibited comparable single-cell performance to that of commercial Pt/C at 0.7 V. Although the Pt loading of the anode with Pd₉₅Pt₅/C was as low as 0.02 mg cm⁻², the specific power (power to mass of Pt in the MEA) of Pd₉₅Pt₅/C was higher than that of Pt/C at 0.7 V. Furthermore, the single-cell performance with Pd₅₀Pt₅₀/C and Pd₇₅Pt₂₅/C as the anode catalyst at 0.4 V was approximately 95% that of the MEA with the Pt/C catalyst. This indicated that a Pd-based catalyst that has an extremely small amount of Pt (only 5 or 50 at.%) can be replaced as an anode electrocatalyst in PEMFC.     

Carbon supported Pt70Co30 electrocatalyst prepared by the formic acid method for the oxygen reduction reaction in polymer electrolyte fuel cells

Carbon supported Pt and Pt₇₀Co₃₀ electrocatalysts for the oxygen reduction reaction (ORR) were prepared by reduction with formic acid and tested in polymer electrolyte fuel cells. In the presence of Co an increase of the Pt particle size was observed in the as-prepared electrocatalyst and no evidence of Pt–Co alloy formation was detected from XRD measurements. Following thermal treatment (TT) at 900 °C of the Pt₇₀Co₃₀/C electrocatalyst, the presence in the XRD pattern of secondary Pt reflexions shifted to higher angles indicated partial alloy formation. The fuel cell performance with the as-prepared Pt₇₀Co₃₀/C electrocatalyst was inferior than that with Pt/C. The electrocatalytic activity increased with a TT of the binary electrocatalyst, and the value of the mass activity of the Pt₇₀Co₃₀/C electrocatalyst thermally treated at 900 °C was only slightly lower than that of Pt/C, notwithstanding the larger metal particle size, about five times that of pure Pt. On the other hand, there was a remarkable increase of the specific activity for the ORR of the Co-containing catalyst after TT at 900 °C with respect to Pt alone, which was ascribed to both the increased metal particle size and alloy formation. At high current densities the performance of PEMFC electrodes decreased with increasing Pt particle size.     

Binary CuPt alloy nanoparticles assembled on reduced graphene oxide-carbon black hybrid as efficient and cost-effective electrocatalyst for PEMFC

Addressed herein is the synthesis of binary CuPt alloy nanoparticles (NPs), their assembly on reduced graphene oxide (rGO), Vulcan XC72 (VC) and their hybrid (rGO-VC) to be utilized as electrocatalysts for fuel cell reactions (HOR and ORR) in acidic medium and PEMFC tests. The synthesis of nearly-monodisperse Cu₄₅Pt₅₅ alloy NPs was achieved by using a chemical reduction route comprising the reduction of commercially available metal precursors in a hot surfactant solution. As-synthesized Cu₄₅Pt₅₅ alloy NPs were then assembled on three support materials, namely rGO, VC and rGO-VC) via liquid phase self-assembly method. After the characterization, the electrocatalysts were prepared by mixing the yielded materials with Nafion and their electrocatalysis performance was investigated by studying CV and LSV for HOR and ORR in acidic medium. Among the three electrocatalysts tested, Cu₄₅Pt₅₅/rGO-VC hybrid showed the highest catalytic activity with ECSA of 119 m² g⁻¹ and mass activity of 165 mA mg⁻¹_Pt. After the evaluation of electrochemical performance of the three prepared electrocatalysts, their performance was then evaluated in fuel cell conditions. In similar to electrochemical activities, the Cu₄₅Pt₅₅/rGO-VC hybrid electrocatalyst showed a superior fuel cell performance and power output by providing a maximum power of 480 mW cm⁻² with a relatively low Pt loading (0.28 mg cm⁻²). Additionally, the Cu₄₅Pt₅₅/rGO-VC hybrid electrocatalyst exhibited substantially better activity as compared to Pt/rGO-VC electrocatalyst. Therefore, the present study confirmed that alloying Pt with Cu enhances the catalytic activity of Pt metal along with the help of beneficial features of rGO-VC hybrid support material. It should be noted that this is the first example of studying PEMFC performance of CuPt alloy NPs supported on rGO, VC and rGO-VC hybrid.     

Study of membrane electrode assemblies for PEMFC,with cathodes prepared by the electrospray method

The electrospray deposition of platinum supported on carbon (Pt/C) particles has been used for the preparation of electrodes for proton exchange membrane fuel cells (PEMFCs). The departing suspensions contain the Pt/C electrocatalyst together with an ionomer (Nafion^®) and a solvent. Two types of solvent have been used, isopropanol and a mixture of butylacetate, ethanol and glycerol (BEG). The microscopic characterisation of electrosprayed films shows the electrospray deposited Pt/C films with a dendritic morphology. XPS analysis of the films reflects changes in the ionomer component after electrospray deposition. A decrease in the signal corresponding to backbone chain (CF₂) is observed on the films deposited with the low evaporation temperature solvent (isopropanol), indicating some disruption of ionomer chains during the electrospray process. With high evaporation temperature solvent (BEG), the disruption effect seems less acute. Membrane electrode assemblies were prepared with the electrosprayed electrodes as cathodes. Good general performance is encountered, comparable with standard commercial cathodes. Electrosprayed electrodes prepared from high evaporation temperature solvent (BEG) show a higher surface specific area. The internal resistance is something higher for MEAs with electrosprayed cathodes. The long term stability test shows a performance loss of about 10 μV h⁻¹ over 700 h continuous testing.     

Carbon supported Pt hollow nanospheres as anode catalysts for direct borohydride-hydrogen peroxide fuel cells

The carbon supported Pt hollow nanospheres were prepared by employing cobalt nanoparticles as sacrificial templates at room temperature in aqueous solution and used as the anode electrocatalyst for direct borohydride-hydrogen peroxide fuel cell (DBHFC). The physical and electrochemical properties of the as-prepared electrocatalysts were investigated by transmission electron microscopy (TEM), X-ray diffraction (XRD), cyclic voltammetry (CV), chronoamperometry (CA), chronopotentiometry (CP) and fuel cell test. The results showed that the carbon supported Pt nanospheres were coreless and composed of discrete Pt nanoparticles with the crystallite size of about 2.8 nm. Besides, it has been found that the carbon supported Pt hollow nanospheres exhibited an enhanced electrocatalytic performance for BH₄⁻ oxidation compared with the carbon supported solid Pt nanoparticles, and the DBHFC using the carbon supported Pt hollow nanospheres as electrocatalyst showed as high as 54.53 mW cm⁻² power density at a discharge current density of 44.9 mA cm⁻².     

Platinum/vivianite bifunction catalysts for DMFC

Bi-functional catalysts are used to solve the poisoning problem caused by carbon monoxide (CO) which is the intermediate of direct methanol fuel cells (DMFCs). Flower-like vivianite (Fe₃(PO₄)₂·8H₂O) spheres with diameter around 10 μm are originally used as supports of Pt to form bifunction catalysts. The cyclic voltammetry in 1 M H₂SO₄ indicates that the electrochemical surface area (ECSA) of Pt reduced on as-prepared vivianite (Pt/Vi) was 105, greater than 91 m² g⁻¹ for the commercial Pt/C. Besides, Pt/Vi reveals the less CO poisoning effects, including the greater mass activity in methanol oxidation and the lower onset potential in CO-stripping than Pt/C. These excellent performances on electrolyzes are related to the chemical state of Fe³⁺ and the coexistence of Pt⁰ and Pt²⁺ in Pt/Vi. The former activates the water and yields Fe-OH_ads at lower potential and the latter may offer an easy way of electron transition.     

An effective electrocatalyst based on platinum nanoparticles supported with graphene nanoplatelets and carbon black hybrid for PEM fuel cells

A facile synthesis at room temperature and at solid-state directly on the support yielded small, homogeneous and well-dispersed Pt nanoparticles (NPs) on CB-carbon black, GNP-graphene nanoplatelets, and CB-GNP-50:50 hybrid support. Synthesized Pt/CB, Pt/GNP and Pt/CB:GNP NPs were used as electrocatalysts for polymer electrolyte membrane fuel cell (PEMFC) reactions. HRTEM results displayed very small, homogeneous and well-dispersed NPs with 1.7, 2.0 and 4.2 nm mean-diameters for the Pt/CB-GNP, Pt/GNP and Pt/CB electrocatalysts, respectively. Electrocatalysts were also characterized by RAMAN, XRD, BET and CV techniques. ECSA values indicated better activity for graphene-based supports with 19 m² g⁻¹_Pt for Pt/GNP and 55 m² g⁻¹_Pt for Pt/CB-GNP compared to 10 m² g⁻¹_Pt for Pt/CB. Oxygen reduction reaction (ORR) studies and fuel cell tests were in parallel with these results where highest maximum power density of 377 mW cm⁻² was achieved with Pt/CB-GNP hybrid electrocatalyst. Both fuel cell and ORR studies for Pt/CB-GNP indicated better dispersion of NPs on the support and efficient fuel cell performance that is believed to be due to the prevention of restacking of GNP by CB. To the best of our knowledge, Pt/GNP and Pt/CB-GNP electrocatalysts are the first in literature to be synthesized with the organometallic mild synthesis method using Pt(dba)₃ precursor for the PEMFC applications.     

Electrospun Pt/TiO2 hybrid nanofibers for visible-light-driven H2 evolution

One-dimensional (1D) Pt/TiO₂ hybrid nanofibers (HNFs) with different concentrations of Pt were fabricated by a facile two-step synthesis route combining an electrospinning technique and calcination process. X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HRTEM) results showed that the Pt nanoparticles (NPs) with the size of 5–10 nm were well dispersed in the TiO₂ nanofibers (NFs). Further investigations from the UV–Vis diffuse reflectance (DR) and X-ray photoelectron spectroscopy (XPS) analysis revealed that some Pt ions were incorporated into the TiO₂ lattice as Pt⁴⁺ state, which contributed to the visible light absorption of TiO₂ NFs. Meanwhile, the Pt²⁺ ions existing on the surface of Pt NPs resulted in the formation of Pt–O–Ti bond at Pt NPs/TiO₂ NFs interfaces that might serve as an effective channel for improving the charge transfer. The as-electrospun Pt/TiO₂ HNFs exhibited remarkable activities for photocatalytic H₂ evolution under visible light irradiation in the presence of l-ascorbic acid as the sacrificial agent. In particular, the optimal HNFs containing 1.0 at% Pt showed the H₂ evolution rate of 2.91 μmol h⁻¹ and apparent quantum efficiency of 0.04% at 420 nm by using only 5 mg of photocatalysts. The higher photocatalytic activity could be ascribed to the appropriate amount of Pt ions doping and excellent electron-sink effect of Pt NPs co-catalysts.