CN114318412A - Limited-domain N-doped Fe nano-particles and preparation method and application thereof - Google Patents
Limited-domain N-doped Fe nano-particles and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the field of preparation and application of nanoparticles, and provides a limited-domain N-doped Fe nanoparticle and a preparation method and application thereof. The size of the limited-domain N-doped Fe nano-particles is about 3-10 nm, and the limited-domain N-doped Fe nano-particles grow in an amorphous carbon matrix and have high dispersibility. The preparation method of the nano-particles is simple and rapid, the whole preparation process only needs tens of minutes, namely, firstly, the pulse laser deposition technology is combined with the rapid annealing treatment to obtain the limited-area Fe nano-particles, and then, the N is adopted2The radio frequency plasma technology realizes controllable N doping of the nano particles. Electrochemical measurements show thatThe N-doped Fe nano-particles show enhanced activity and stability of electrocatalytic water decomposition to generate Oxygen (OER), and only low overpotential of 246 mV is needed to drive 10mA cm in a 1M KOH solution‑2The current density of (1). The invention not only provides a simple and rapid method for preparing the metal nano-particles with the limited domain structure and controllable N doping, but also greatly promotes the development of the OER electrocatalyst.
Description
Technical Field
The invention relates to the field of preparation and application of nanoparticles, in particular to a limited-area nitrogen-doped iron (N-doped Fe) nanoparticle and a preparation method and application thereof.
Background
The electrocatalytic Oxygen Evolution Reaction (OER) is an important anodic half-reaction involving many important energy conversion and storage systems, such as electrolytic water evolution of hydrogen, carbon dioxide reduction, nitrogen conversion to ammonia, hydrogen peroxide synthesis, rechargeable metal air batteries, etc. The catalytic efficiency of OER directly affects the development of electrochemical technology. The urgent need for large-scale application of OER electrocatalysts in the past few years has prompted a wide search for low-cost, abundant-source iron-based electrocatalysts. However, the OER performance of iron-based electrocatalysts needs to be further improved to replace noble metal-based electrocatalysts. N doping is one of the most effective strategies to increase the OER activity of iron-based electrocatalysts. It is reported that the d-band state density of Fe varies with the formation of Fe — N bond, so that the catalytic activity of Fe-based OER electrocatalyst can be greatly improved.
On the other hand, reducing the size of the catalyst is also an effective means to increase the intrinsic activity of the electrocatalyst. Thus, during the last decades, nanoparticle electrocatalysts have attracted great interest due to their high specific surface area and catalytic activity. However, nanoparticle electrocatalysts often suffer from agglomeration problems during the catalytic process, which results in a significant reduction in catalytic performance and stability. Confining nanoparticles in a solid matrix is an ideal way to inhibit their agglomeration and property decay. Furthermore, the highly active nanoparticles in the solid matrix may also achieve a "limited catalysis" effect, which will effectively tune the catalytic performance. It is noteworthy that carbon offers an ideal choice for a solid matrix due to its high conductivity for fast electron transport. However, achieving confined-domain growth of Fe-based nanoparticles in a carbon matrix and their controllable N-doping is currently still a huge challenge.
Disclosure of Invention
The invention aims to provide a limited-domain N-doped Fe nano particle, a preparation method and application thereof, and solves the problems in the prior art at least to a certain extent.
The size of the limited-domain N-doped Fe nano-particles is about 3-10 nm, the limited-domain growth is carried out in an amorphous carbon matrix, and the distribution density is 0.5-2 multiplied by 1011cm2。
The invention provides a preparation method of a limited-domain N-doped Fe nano particle, which comprises the following steps:
depositing Fe by adopting a pulse laser deposition technology and carrying out annealing treatment to obtain a limited-area Fe nano particle;
using radio frequency plasma technology to make N2Reacting with the limited-domain Fe nano-particles to obtain limited-domain N-doped Fe nano-particles.
Preferably, the preparation method of the limited-domain N-doped Fe nanoparticle specifically comprises the following steps:
bonding the iron target and the carbon target surface by using silver colloid to form a composite target material of two materials, and ablating the composite target material by using laser under a vacuum condition to deposit carbon and iron on a substrate; after deposition, annealing at 500-700 ℃ under the protection of inert gas to obtain the limited-area Fe nano particles;
putting the limited domain type Fe nano particles into a reactor of a radio frequency plasma chemical vapor deposition system, and adding N2And (4) processing in the atmosphere to obtain the limited-area N-doped Fe nano particles.
Preferably, the vacuum degree under the vacuum condition is 1-5 multiplied by 10-8And Torr, wherein the wavelength of the laser is 248nm, and the deposition time is 5-10 minutes.
Preferably, the substrate is a glassy carbon sheet.
Preferably, the inert gas is Ar gas.
Preferably, the annealing time is 5-10 minutes.
Preferably, the power of the radio frequency plasma is 100W, and the processing time is 2-10 minutes.
The limited domain type N-doped Fe nano-particles provided by the invention can be used as a high-efficiency OER electrocatalyst for water electrocatalytic decomposition reaction.
The invention has the technical effects that: (1) the preparation method of the limited-domain N-doped Fe nano-particles is simple and quick, the whole preparation process only needs tens of minutes, and the N-doped concentration can be simply and conveniently controlled through radio frequency time; (2) in the limited-domain N-doped Fe nano-particles, the Fe nano-particles grow in a carbon matrix in a limited domain mode, so that the stability of the nano-particles is effectively ensured, and the Fe nano-particles have uniform and controllable N element doping; (3) the confined-domain N-doped Fe nano-particles have excellent activity and stability in the aspect of electrocatalytic OER.
Drawings
Fig. 1 is a Transmission Electron Microscope (TEM) characterization of the confined Fe nanoparticles and N-doped Fe nanoparticles prepared according to one embodiment of the present invention.
Fig. 2 is a schematic structural diagram of a domain-restricted nanoparticle prepared according to an embodiment of the present invention.
Fig. 3 is an X-ray photoelectron spectroscopy (XPS) characterization of the confined Fe nanoparticles and the N-doped Fe nanoparticles prepared according to an embodiment of the present invention.
Fig. 4 is a graph of electrocatalytic OER performance of the domain-limited Fe nanoparticles and N-doped Fe nanoparticles prepared according to one embodiment of the present invention.
FIG. 5 shows the stability test results of the electrocatalytic OER of the confined Fe nanoparticles and the N-doped Fe nanoparticles prepared by the present invention.
Detailed Description
The technical solutions and advantages of the present invention will be described in detail below with reference to the accompanying drawings and specific examples, which are intended to help the reader to better understand the essence of the present invention, but should not be construed as limiting the scope of the present invention.
The limited-domain N-doped Fe nanoparticle provided by the invention can comprise a substrate and a limited-domain N-doped Fe nanoparticle attached to the substrate in a thin film form; the size of the limited-domain N-doped Fe nano particles is about 3-10 nm, and the limited domains of the limited-domain N-doped Fe nano particles grow in an amorphous carbon matrix; the limited-domain N-doped Fe nano-particles have high dispersity, and the distribution density of the limited-domain N-doped Fe nano-particles is about 0.5-2.0 multiplied by 1011 cm2。
The preparation method of the limited-domain N-doped Fe nano-particles provided by the invention comprises the following steps of:
step (1), providing a clean substrate: before growth, firstly polishing a commercial glassy carbon film substrate for 2-5 hours, and then thoroughly cleaning the substrate with deionized water, ethanol and the like under the action of strong ultrasound to obtain a clean surface for deposition;
step (2), adopting a pulse laser deposition technology and combining with rapid annealing treatment to obtain the limited-area Fe nano particles: firstly, manufacturing a target material, wherein the target material consists of a carbon target with the radius of 5-20 mm and an iron rectangular target with the length of 5-15 mm; bonding the iron target and the carbon target surface by using silver adhesive to form a composite target material of two materials; then, a commercial glassy carbon sheet is used as a deposition substrate, and the deposition substrate is placed in ultrahigh vacuum (1-5 multiplied by 10)-8Torr) and ablating the target material for 5-10 minutes by using 10 Hz laser (248 nm); during deposition, the target is rotated around a central axis at a constant speed; after deposition, under the flowing protection of Ar gas of 100 sccm, rapidly annealing the deposited sample at 500-700 ℃ for 5-10 minutes to obtain the limited-area Fe nanoparticles;
step (3), using N2The radio frequency plasma technology realizes controllable N doping of Fe nanoparticles: putting the limited-area Fe nano particles into a reactor of a radio frequency plasma chemical vapor deposition system, and using N2Cleaning the reactor for three times; then, treating the mixture in a radio frequency plasma reactor with the power of 100W for 2-10 minutes to obtain a limited-area N-doped Fe nano particle; the pressure in the reactor was kept at about 10Torr throughout the process, and nitrogen (purity: 99.999%) was flowed at a rate of 40 sccm.
Several exemplary embodiments are described below.
Example 1:
before growth, firstly polishing a commercial glassy carbon film substrate for 2-5 hours, and then thoroughly cleaning with deionized water, ethanol and the like under the action of strong ultrasound to obtain a clean surface for deposition. And manufacturing a target material, wherein the target material consists of a carbon target with the radius of 20mm and an iron rectangular target with the length of 15mm, and the iron target and the carbon target are bonded by silver colloid to form the composite target material of the two materials. Then, a commercial glass carbon plate is used as a deposition substrate, and the substrate is placed in ultrahigh vacuum (5 multiplied by 10)-8Torr) the target was ablated with a 10 Hz laser (248 nm) for 5 minutes. During deposition, the target is rotated around a central axis at a constant speed. After deposition, under the flowing protection of Ar gas of 100 sccm, the deposited sample is quickly annealed for 6 minutes at 600 ℃ to obtain the limited-area Fe nano-particles. Putting the limited domain type Fe nano particles into a reactor of a radio frequency plasma chemical vapor deposition system, and using N2The reactor was washed three times. And then, processing the mixture in a radio frequency plasma reactor with the input power of 100W for 6 minutes to obtain the limited-area N-doped Fe nano-particles. The pressure in the reactor was kept at about 10Torr throughout the process, and nitrogen (purity: 99.999%) was flowed at a rate of 40 sccm. The confined-domain N-doped Fe nanoparticles obtained in this example were labeled N-Fe @6 NPs.
Example 2:
before growth, firstly polishing a commercial glassy carbon film substrate for 2-5 hours, and then thoroughly cleaning with deionized water, ethanol and the like under the action of strong ultrasound to obtain a clean surface for deposition. And manufacturing a target material, wherein the target material consists of a carbon target with the radius of 20mm and an iron rectangular target with the length of 15mm, and the iron target and the carbon target are bonded by silver colloid to form the composite target material of the two materials. Then, a commercial glass carbon plate is used as a deposition substrate, and the substrate is placed in ultrahigh vacuum (5 multiplied by 10)-8Torr) the target was ablated with a 10 Hz laser (248 nm) for 6 minutes. During deposition, the target is rotated around a central axis at a constant speed. After deposition, under the flow protection of 100 sccm Ar gas, the deposited sample is rapidly annealed for 5 minutes at 500 ℃ to obtain the limited-area Fe nano-particles. Putting the limited domain type Fe nano-particles into a reactor of a radio frequency plasma chemical vapor deposition system,with N2The reactor was washed three times. And then, treating the mixture in a radio frequency plasma reactor with the input power of 100W for 10 minutes to obtain the limited-area N-doped Fe nano-particles. The pressure in the reactor was kept at about 10Torr throughout the process, and nitrogen (purity: 99.999%) was flowed at a rate of 40 sccm. The confined-domain N-doped Fe nanoparticles obtained in the present example were labeled as N-Fe @10 NPs.
Example 3:
before growth, firstly polishing a commercial glassy carbon film substrate for 2-5 hours, and then thoroughly cleaning with deionized water, ethanol and the like under the action of strong ultrasound to obtain a clean surface for deposition. And manufacturing a target material, wherein the target material consists of a carbon target with the radius of 20mm and an iron rectangular target with the length of 15mm, and the iron target and the carbon target are bonded by silver colloid to form the composite target material of the two materials. Then, a commercial glass carbon plate is used as a deposition substrate, and the substrate is placed in ultrahigh vacuum (5 multiplied by 10)-8Torr) the target was ablated with a 10 Hz laser (248 nm) for 5 minutes. During deposition, the target is rotated around a central axis at a constant speed. After deposition, under the flowing protection of Ar gas of 100 sccm, the deposited sample is quickly annealed for 10 minutes at 600 ℃ to obtain the limited-area Fe nano-particles. Putting the limited domain type Fe nano particles into a reactor of a radio frequency plasma chemical vapor deposition system, and using N2The reactor was washed three times. And then, processing the mixture in a radio frequency plasma reactor with the input power of 100W for 2 minutes to obtain the limited-area N-doped Fe nano-particles. The pressure in the reactor was kept at about 10Torr throughout the process, and nitrogen (purity: 99.999%) was flowed at a rate of 40 sccm. The confined-domain N-doped Fe nanoparticles obtained in the present example were labeled as N-Fe @2 NPs.
The size of the limited-domain N-doped Fe nanoparticles prepared in examples 1 to 3 is about 3 to 10 nm, and the limited domain of the N-doped Fe nanoparticles is grown in an amorphous carbon matrix; the nanoparticles have high dispersibility and a distribution density of about 2.0 × 1011cm2(ii) a The amorphous carbon matrix is attached to a commercial glassy carbon substrate.
The prepared N-doped confinement type Fe nano-particles can be used as an OER electro-catalyst for water electrocatalytic decomposition reaction. And testing the electrocatalytic OER performance of the N-doped confinement type Fe nano-particles, wherein the testing technical scheme is as follows: adopting a three-electrode system of an electrochemical workstation to test the electrocatalysis performance, wherein a graphite rod electrode is adopted as a counter electrode, and a saturated calomel electrode is adopted as a reference electrode; testing by using N-doped confined-domain Fe nanoparticles growing on a commercial glassy carbon substrate as a working electrode and using 1M KOH aqueous solution as electrolyte; measuring a polarization curve by adopting a linear sweep voltammetry method, wherein the sweep rate is set to be 0.005V/s; all measured potentials are converted to reversible hydrogen electrode potentials.
Fig. 1a shows a low resolution TEM image of uniform Fe nanoparticles with high surface density in a carbon matrix. The carbon matrix remains in the amorphous phase. The average size of the Fe nanoparticles was about 7 nm and the surface density was about 2.0X 1011 cm-2. Fig. 1b shows Selected Area Electron Diffraction (SAED) patterns of nanoparticles and simulated electron diffraction patterns generated by TEM Java electron microscope simulation software (JEMS), and it can be found that the SAED patterns of Fe nanoparticles actually measured are very consistent with the simulated patterns. It can therefore be concluded that the crystalline phase of Fe nanoparticles is cubic metallic iron. FIG. 1c shows an atomic diagram of cubic metallic iron. High resolution tem (hrtem) images of the individual Fe nanoparticles in fig. 1d show that they have good crystallinity with a lattice spacing (0.203 nm) consistent with the (111) crystallographic planes of cubic Fe. FIG. 1e shows a warp of N2Low resolution TEM images of N-doped Fe nanoparticle samples (denoted as N-Fe @6 NP) prepared after 6 minutes of rf plasma treatment, where homogeneous nanoparticles and amorphous carbon matrix are shown. Moreover, the appearance, size and surface density of the N-doped silicon nitride film are not obviously changed compared with those before N-doping. FIG. 1f shows Selected Area Electron Diffraction (SAED) patterns of nanoparticles and simulated electron diffraction patterns generated by TEM Java Electron microscope simulation software (JEMS). The crystal phase of the N-doped Fe nano-particles can be inferred to be hexagonal structure Fe3N (space group P6)322) The atomic structure diagram is shown in 1 h. The lattice fringes in FIG. 1g with a spacing of 0.21 nm can be labeled as Fe3N (111) crystal face.
Fig. 2 is a schematic diagram of the structure of the domain-restricted nanoparticles, which can clearly show the structure of the synthesized material, and the nanoparticles are domain-restricted grown in an amorphous carbon matrix attached to a commercial glassy carbon substrate.
Fig. 3 shows XPS spectra of the prepared Fe nanoparticles and N-doped Fe nanoparticles, and the corresponding elements of C, Fe, and N can be clearly identified. FIG. 3a shows that for pure Fe nanoparticles, the C-C bond is mainly at 284.8 eV. However, for the N-doped Fe nanoparticles, in addition to the C-C bond, a peak of the C-N bond also appears at 286.1 eV, indicating that the N element is successfully doped into the carbon matrix. Figure 3b shows a double peak of zero valent iron at 707.6 eV and 720.6 eV for Fe nanoparticles, indicating the presence of metallic Fe. However, after N doping, the state of Fe shows a great change to a mixed state of ferrous and ferric iron. The three peaks of the state of N from low to high binding energy in FIG. 3c are attributed to the pyridine-N, Fe-N species and the graphite-N species, respectively. The Fe-N bond can be attributed to Fe3The existence of N component. In general, we pass N2The short-time treatment of the rf plasma successfully and rapidly dopes N atoms into the iron nanoparticles and the carbon matrix.
Fig. 4 shows a graph of electrocatalytic OER performance for the confined Fe nanoparticles and the N-doped Fe nanoparticles. Samples of different plasma treatment times (N-Fe @2 NPs obtained at 2 minutes and N-Fe @10 NPs obtained at 10 minutes), commercial IrO2And pure N-doped carbon matrix (NC) were also used for comparison. FIG. 4a shows that N-Fe @6NPs require a very low overpotential (246 mV) to drive 10mA cm-2Current density of (2) and commercial IrO2(304 mV) compared, it showed superior OER capability. The OER activity of NC was poor, indicating that the OER active site of N-Fe @6NPs is a nanoparticle rather than a carbon matrix. When the current density is 10mA cm-2In the meantime, the overpotential of the N-doped Fe nanoparticles is much lower than that of pure Fe nanoparticles (316 mV), indicating that the N-doping greatly improves the electrocatalytic OER performance of the Fe nanoparticles. Notably, N-Fe @6NPs exhibited better performance than N-Fe @2 NPs (256 mV) and N-Fe @10 NPs (264 mV). That is, the OER activity of N-doped Fe nanoparticles increased and then decreased with increasing N content, indicating that too much or too little N doping is detrimental to the improvement of catalytic activity (FIG. 4 b). To further study the OER performance of the different samples, the electrocatalytic reaction kinetics were further evaluated by Tafel slope. The results indicate that N-Fe @6NPs are the lowest of these samples (50 mV dec)-1) Indicating that N-Fe @6NPs have more favorable reaction kinetics for OER. In addition, the OER characteristics of the different catalysts were analyzed from the viewpoint of electron conductivity, which is considered as a key parameter of OER. EIS measurements were made at a voltage of 1.54V. As shown in fig. 4c, the fitted EIS results show that N-Fe @6NPs shows the lowest charge transfer resistance (15 Ω), reflecting its excellent electron transfer capability. Furthermore, electrochemically active surface area (ECSA) is also another critical factor in OER performance. As can be seen from FIG. 4d, N-Fe @6NPs exhibited the largest C compared to other catalystsdlValue (1.19 mF cm-2) This is also an important reason for its high catalytic activity. In summary, the above results demonstrate that the OER activity of Fe nanoparticles can be greatly improved by introducing N doping.
Fig. 5a shows the LSV curve before and after 1000 CV cycles. It can be found that the LSV curve does not vary much, which reflects the good stability of the sample. In addition, long term durability testing of the samples showed that at 10mA cm-2The potential value was found to be almost unchanged by measuring continuously 10 h by chronopotentiometry at a fixed current density of (2) (as shown in FIG. 5 b), indicating that N-Fe @6NPs have excellent durability. To further understand the OER stability, XPS after long term OER testing of N-Fe @6NPs was characterized as shown in figure 5 c. No new peaks of Fe appeared, indicating that N-Fe @6NPs have excellent corrosion resistance. In addition, the lattice structure and morphology of the N-Fe @6NPs after long term OER testing was also unchanged (fig. 5 d). In short, the results indicate that N-Fe @6NPs are a very stable OER electrocatalyst.
The confinement type N-doped Fe nano-particle has excellent electrocatalytic performance, and mainly has the advantages that due to the unique confinement structure and the synergistic effect of N doping, the electrochemical surface area is improved, and the conductivity is improved.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (9)
1. The confined-domain N-doped Fe nano-particles are characterized in that the size of the confined-domain N-doped Fe nano-particles is 3-10 nm, the confined-domain N-doped Fe nano-particles grow in an amorphous carbon matrix, and the distribution density is 0.5-2 multiplied by 1011cm2。
2. A preparation method of a limited-domain N-doped Fe nanoparticle comprises the following steps:
depositing Fe by adopting a pulse laser deposition technology and carrying out annealing treatment to obtain a limited-area Fe nano particle;
using radio frequency plasma technology to make N2Reacting with the limited-domain Fe nano-particles to obtain limited-domain N-doped Fe nano-particles.
3. The method according to claim 2, wherein the preparation method of the domain-limited N-doped Fe nanoparticles comprises the following steps:
bonding the iron target and the carbon target surface by using silver colloid to form a composite target material of two materials, and ablating the composite target material by using laser under a vacuum condition to deposit carbon and iron on a substrate; after deposition, annealing at 500-700 ℃ under the protection of inert gas to obtain the limited-area Fe nano particles;
putting the limited domain type Fe nano particles into a reactor of a radio frequency plasma chemical vapor deposition system, and adding N2And (4) processing in the atmosphere to obtain the limited-area N-doped Fe nano particles.
4. The method according to claim 3, wherein the degree of vacuum of the vacuum condition is 1 to 5 x 10-8And Torr, wherein the wavelength of the laser is 248nm, and the deposition time is 5-10 minutes.
5. The method of claim 3, wherein the substrate is a glass carbon sheet.
6. The method of claim 3, wherein the inert gas is Ar gas.
7. The method of claim 3, wherein the annealing time is 5 to 10 minutes.
8. The method of claim 3, wherein the RF plasma has a power of 100W and a processing time of 2-10 minutes.
9. Use of the confined-domain N-doped Fe nanoparticles of claim 1 as an OER electrocatalyst.
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