Method for preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technique
By treating oxide precursor solutions with liquid-phase laser irradiation technology, pure and uniform zero-dimensional oxide nanoparticles were prepared, solving the preparation problems in existing technologies and making them suitable for optoelectronic, energy storage and catalysis fields.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- NORTHWESTERN POLYTECHNICAL UNIV
- Filing Date
- 2024-07-15
- Publication Date
- 2026-06-26
AI Technical Summary
Existing technologies struggle to efficiently prepare pure, uniformly sized zero-dimensional oxide nanoparticles, especially white oxides and multi-component oxides, and conventional methods suffer from insufficient particle uniformity.
Zero-dimensional oxide nanoparticles were prepared by treating oxide precursor solutions with liquid-phase laser irradiation technology, using a high-energy laser with a wavelength of 1064 nm to instantaneously melt the oxide precursors in the solvent, and then separating the solvent by a rapid rotary evaporation method.
We can obtain pure, uniformly sized zero-dimensional oxide nanoparticles suitable for various oxides, which maintain small size and uniformity in solvents, making them applicable to optoelectronic, energy storage and catalysis fields.
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Figure CN118894504B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of materials preparation technology, and specifically relates to a method for preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology. Background Technology
[0002] Zero-dimensional nanomaterials refer to materials with small particle sizes, typically below 10 nm. The small particle size of zero-dimensional nanomaterials leads to an increased proportion of atoms on the particle surface and a significant increase in surface state density, giving them unique properties that differ from large-sized materials, such as quantum size effect, quantum tunneling effect, and quantum confinement effect. These unique optical, electrical, and magnetic properties make zero-dimensional nanomaterials show application potential in many fields such as biology, medicine, energy, and catalysis.
[0003] Zero-dimensional nanomaterials are diverse, mainly encompassing elemental metals (including Pt, Au, and Ag nanoclusters), carbon quantum dots (functionalized carbon dots), and oxide ultrafine nanoparticles. Among these materials, oxides possess multifunctionality due to their abundance of characteristic metals, and variations in oxygen sites also significantly contribute to improving their properties. However, the inherent high thermal stability of oxides makes the preparation of zero-dimensional oxide ultrafine particles quite challenging.
[0004] There are two main conventional methods for preparing zero-dimensional nanomaterials: one is the bottom-up wet chemical method, which has the advantage of controllable particle size uniformity, but it has high requirements for the types of materials and requires ligands throughout the preparation process, making subsequent purification complex and difficult to obtain ligand-free zero-dimensional nanomaterials; the other is the top-down strategy, which mainly uses external energy (including sound, light, electricity, and force) to process large-sized materials to obtain small-sized zero-dimensional materials. This strategy has the advantage of fewer restrictions on the types of materials and does not require the addition of ligands, but due to the potential for uneven energy absorption within the material, its particle uniformity needs further improvement. It is evident that the above-mentioned existing methods have certain technical defects in preparing zero-dimensional oxide nanoparticles, thus affecting the application of zero-dimensional oxide nanomaterials. Therefore, developing a new method for preparing zero-dimensional oxide nanomaterials is of great significance. Summary of the Invention
[0005] To address the shortcomings of the existing technologies, this invention provides a method for preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology. This invention provides a fast and universally applicable method for preparing zero-dimensional oxide nanoparticles, obtaining pure zero-dimensional oxide nanoparticles with uniform particle size, and overcoming the technical defects of existing preparation methods.
[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:
[0007] The reactants in this invention are only oxide precursors. The oxide precursors are dispersed in a solvent, and the target product is obtained by liquid phase laser irradiation technology. Compared with the prior art, no new impurities are introduced during the preparation process, so the obtained zero-dimensional oxide nanoparticle product is pure. In addition, the zero-dimensional oxide nanoparticles have a uniform particle size distribution, which is mainly due to the fact that laser melting treatment solves the problem of particle agglomeration.
[0008] A method for preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology includes the following steps:
[0009] The oxide precursor was ground to a particle size of micrometers and then dispersed in a solvent to obtain an oxide dispersion.
[0010] After irradiating the oxide dispersion with liquid phase laser irradiation technology, the solvent was separated to obtain zero-dimensional oxide nanoparticles.
[0011] Preferably, the oxide precursor is a multi-component oxide or a non-white binary oxide. White binary oxides are not well prepared using liquid-phase laser irradiation technology because white substances easily reflect laser light at a wavelength of 1064 nm, making it difficult for the laser to act on the material, thus making preparation impossible. White multi-component oxides can also be prepared using liquid-phase laser irradiation technology, but the products are of poor quality and have poor particle size uniformity.
[0012] Preferably, the mass ratio of the oxide precursor to the volume ratio of the solvent in the oxide dispersion is 0.2–1.5 mg / mL.
[0013] Preferably, the laser emission wavelength of the liquid phase laser irradiation technology is 1064nm, and the laser irradiation range is 1.3cm.
[0014] Preferably, the irradiation conditions are: room temperature and laser irradiation energy of 1.2-2.0 J for 1-10 min; the room temperature range is 15℃-45℃. Different temperatures and laser irradiation energies will affect the preparation of zero-dimensional oxide nanoparticles. These conditions were obtained through screening in this application.
[0015] Preferably, the solvent is a non-alcoholic polar solvent, and the oxide reacts slowly or not at all in alcoholic solvents.
[0016] Preferably, the solvent is selected from acetone, N,N'-dimethylformamide, dimethyl sulfoxide, dioxane, or ethylene glycol dimethyl ether.
[0017] Preferably, the grinding method is ball milling, with a ball milling speed of 300-600 rpm and a ball milling time of 8-20 h.
[0018] Preferably, the method for separation and dissolution is vacuum distillation.
[0019] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0020] 1. The principle of preparing zero-dimensional oxide nanoparticles using liquid phase laser irradiation technology in this invention is as follows: 1064nm wavelength laser has the characteristics of high energy and strong heating. Under the high laser irradiation energy of 1.2-2.0J, the instantaneous high temperature generated melts the oxide precursor. The oxide in the high temperature molten state rapidly condenses into nanoscale ultrafine particles in the solvent. This method is also applicable to common non-white oxide materials.
[0021] 2. This invention rapidly and controllably prepares a series of binary or multi-component oxide zero-dimensional ultrafine nanoparticle colloidal solutions under 1064nm wavelength pulsed laser irradiation, covering all non-white oxides. (white oxide and 1064nm excitation) (Light does not have an effect) Furthermore, the range of solvents has been expanded to include non-alcoholic polar solvents, making the preparation method universally applicable.
[0022] 3. The zero-dimensional oxide nanoparticles obtained by the preparation method of the present invention undergo changes in the surface states of the oxides due to laser treatment during the preparation process, and oxygen vacancies are generated by constructing oxygen defects. Oxygen vacancies have a positive effect on the photoelectric, catalytic and energy storage properties of the zero-dimensional oxide nanoparticles.
[0023] 4. The solvent in the colloidal solution prepared by the present invention is separated by rotary evaporation. The entire preparation process is highly pure and free of ligands. After the obtained powder is redispersed in the solvent, it still maintains a small size and uniform distribution. This method is suitable for the mass preparation of zero-dimensional oxide nanoparticles. Attached Figure Description
[0024] Figure 1 a is an optical photograph of the WO3 dispersion from Example 1. Figure 1 b is an optical photograph of the WO3 ultrafine particle colloidal solution of Example 1.
[0025] Figure 2 The images show transmission electron microscopy (TEM) images and particle size distributions of the zero-dimensional WO3 nanoparticles from Example 1.
[0026] Figure 3 This is a transmission electron microscope image of the redispersed zero-dimensional WO3 nanoparticle powder from Example 1.
[0027] Figure 4 The images show X-ray diffraction patterns of zero-dimensional WO3 nanoparticles and WO3 precursors in Example 1 before and after irradiation treatment.
[0028] Figure 5 This is a high-resolution transmission electron microscope image of the zero-dimensional WO3 nanoparticles from Example 1.
[0029] Figure 6 X-ray photoelectron spectra (O 1s orbitals) of zero-dimensional BiVO4 nanoparticles and BiVO4 precursors in Example 4 before and after irradiation treatment.
[0030] Figure 7 The electron paramagnetic resonance spectra of zero-dimensional BiVO4 nanoparticles and BiVO4 precursors in Example 4 before and after irradiation treatment are shown.
[0031] Figure 8 This is a schematic diagram illustrating the principle of preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology.
[0032] Figure 9 The images show transmission electron microscopy (TEM) images and particle size distributions of the zero-dimensional Fe2O3 nanoparticles from Example 2.
[0033] Figure 10 Zero-dimensional NiO as described in Example 3 x Transmission electron microscopy images and particle size distribution of nanoparticles.
[0034] Figure 11 The image shows a transmission electron microscope (TEM) image and particle size distribution of the zero-dimensional BiVO4 nanoparticles from Example 4.
[0035] Figure 12 The image shows a transmission electron microscope (TEM) image and particle size distribution of the zero-dimensional LaFeO3 nanoparticles from Example 5. Detailed Implementation
[0036] The specific embodiments of the present invention are described in detail below, but it should be understood that the scope of protection of the present invention is not limited to the specific embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention. Unless otherwise specified, the experimental methods described in the embodiments of the present invention are conventional methods.
[0037] The method of this invention first obtains colloidal solutions of different zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology, and then obtains different zero-dimensional oxide nanoparticles using rapid rotary evaporation technology. This invention prepares different zero-dimensional oxide nanoparticles in different solvent systems using liquid-phase laser irradiation technology. The oxides involved include binary and multi-component oxides, and it is applicable to various metal and non-metal oxides. By adjusting the laser irradiation parameters, reaction time, and solvent type, the controllable preparation of zero-dimensional oxide nanoparticles is achieved. Furthermore, due to its unique advantage of rapid preparation, it enables the large-scale preparation of zero-dimensional oxide nanoparticles.
[0038] This invention provides a novel and universal strategy for the preparation of zero-dimensional oxide nanomaterials, resulting in pure and uniformly sized zero-dimensional oxide nanomaterials. This will help promote the further development of zero-dimensional oxide materials in the fields of optoelectronics, energy storage, and catalysis.
[0039] The technical solution of this application will be further explained and illustrated below with examples, as detailed below:
[0040] Example 1
[0041] A method for preparing WO3 nanoparticles using liquid-phase laser irradiation technology includes the following steps:
[0042] (1) Place WO3 powder in an agate ball milling jar, add acetone for ball milling, set the ball milling speed to 400 rpm, and the ball milling time to 12 h. After drying, a light green WO3 precursor powder is obtained.
[0043] (2) Weigh 5mg of the WO3 precursor powder from step (1), measure 10mL of acetone, mix and ultrasonically disperse evenly to prepare a WO3 dispersion of 0.2mg / mL, which is yellow-green.
[0044] (3) At room temperature, the WO3 dispersion in step (2) was irradiated for 5 min using an Nd:YAG pulsed laser (pulse frequency 10 Hz, pulse width 8 ns, spot size 13 mm) with the laser energy controlled at 1.2 J to obtain a gray-green WO3 ultrafine particle colloidal solution.
[0045] (4) The WO3 ultrafine particle colloidal solution from step (3) was purified by rapid rotary evaporation and then vacuum dried to obtain a black-green zero-dimensional WO3 nanoparticle powder sample.
[0046] Example 2
[0047] A method for preparing Fe2O3 nanoparticles using liquid-phase laser irradiation technology includes the following steps:
[0048] (1) Fe2O3 powder was placed in an agate ball milling jar, acetone was added for ball milling, the ball milling speed was set to 400 rpm, the ball milling time was 12 h, and after drying, red Fe2O3 precursor powder was obtained.
[0049] (2) Weigh 5mg of Fe2O3 precursor powder from step (1), measure 10mL of acetone, mix and ultrasonically disperse evenly to prepare a 0.2mg / mL Fe2O3 dispersion, which is reddish-brown.
[0050] (3) At room temperature, Fe2O3 dispersion was irradiated for 5 min using an Nd:YAG pulsed laser (pulse frequency 10 Hz, pulse width 8 ns, spot size 13 mm) with laser energy controlled at 1.5 J to obtain a reddish-brown Fe2O3 ultrafine particle colloidal solution.
[0051] (4) The Fe2O3 ultrafine particle colloidal solution from step (3) was purified by rapid rotary evaporation and then vacuum dried to obtain a reddish-brown zero-dimensional Fe2O3 nanoparticle powder sample.
[0052] Example 3
[0053] Zero-dimensional NiO prepared using liquid phase laser irradiation technology x The method for nanoparticles includes the following steps:
[0054] (1) NiO x The powder was placed in an agate ball mill jar, and N,N'-dimethylformamide was added for ball milling. The ball milling speed was set to 400 rpm, and the milling time was 12 hours. After drying, black NiO was obtained. x Precursor powder;
[0055] (2) Weigh 5 mg of NiO from step (1). x Precursor powder, 10 mL of N,N'-dimethylformamide, mixed and ultrasonically dispersed to prepare a 0.2 mg / mL NiO solution. x The dispersion is black.
[0056] (3) At room temperature, the NiO from step (2) was irradiated using an Nd:YAG pulsed laser (pulse frequency 10 Hz, pulse width 8 ns, spot size 13 mm). x Dispersion was carried out for 5 minutes, and the laser energy was controlled at 1.8 J to obtain black NiO. x Ultrafine particle colloidal solution;
[0057] (4) The NiO from step (3) is processed by rapid rotary evaporation. x The ultrafine particle colloidal solution was purified and then vacuum dried to obtain black zero-dimensional NiO. x Nanoparticle powder sample.
[0058] Example 4
[0059] A method for preparing zero-dimensional BiVO4 nanoparticles using liquid-phase laser irradiation technology includes the following steps:
[0060] (1) Place BiVO4 powder in an agate ball milling jar, add dimethyl sulfoxide and ball mill, set the ball milling speed to 400 rpm, and the ball milling time to 12 h. After drying, yellow BiVO4 precursor powder is obtained.
[0061] (2) Weigh 5 mg of BiVO4 precursor powder from step (1), measure 10 mL of dimethyl sulfoxide, mix and ultrasonically disperse evenly to prepare a 0.2 mg / mL BiVO4 dispersion, which is black.
[0062] (3) At room temperature, the BiVO4 dispersion in step (2) was irradiated for 5 min using an Nd:YAG pulsed laser (pulse frequency 10 Hz, pulse width 8 ns, spot size 13 mm) with the laser energy controlled at 1.2 J to obtain a black BiVO4 ultrafine particle colloidal solution.
[0063] (4) The BiVO4 ultrafine particle colloidal solution from step (3) was purified by rapid rotary evaporation and then dried under vacuum to obtain a black zero-dimensional BiVO4 nanoparticle powder sample.
[0064] Example 5
[0065] A method for preparing zero-dimensional LaFeO3 nanoparticles using liquid-phase laser irradiation technology includes the following steps:
[0066] (1) Place LaFeO3 powder in an agate ball milling jar, add ethylene glycol dimethyl ether for ball milling, set the ball milling speed to 400 rpm, and the ball milling time to 12 h. After drying, LaFeO3 precursor powder is obtained.
[0067] (2) Weigh 5mg of the LaFeO3 precursor powder from step (1), measure 10mL of ethylene glycol dimethyl ether, mix and ultrasonically disperse evenly to prepare a 0.2mg / mL LaFeO3 dispersion, which is black.
[0068] (3) At room temperature, the LaFeO3 dispersion in step (2) was irradiated for 5 min using an Nd:YAG pulsed laser (pulse frequency 10 Hz, pulse width 8 ns, spot size 13 mm) with laser energy controlled at 2.0 J to obtain a black BiVO4 ultrafine particle colloidal solution.
[0069] (4) The LaFeO3 ultrafine particle colloidal solution from step (3) was purified by rapid rotary evaporation and then dried under vacuum to obtain a black zero-dimensional LaFeO3 nanoparticle powder sample.
[0070] Comparative Example 1
[0071] The method for preparing WO3 nanoparticles using liquid-phase laser irradiation technology is the same as the preparation steps in Example 1, except that the laser energy is replaced by 1.0 J instead of 1.2 J, and includes the following steps:
[0072] (1) Place WO3 powder in an agate ball milling jar, add acetone for ball milling, set the ball milling speed to 400 rpm, and the ball milling time to 12 h. After drying, a light green WO3 precursor powder is obtained.
[0073] (2) Weigh 5mg of the WO3 precursor powder from step (1), measure 10mL of acetone, mix and ultrasonically disperse evenly to prepare a WO3 dispersion of 0.2mg / mL, which is yellow-green.
[0074] (3) At room temperature, the WO3 dispersion in step (2) was irradiated for 5 min using an Nd:YAG pulsed laser (pulse frequency 10 Hz, pulse width 8 ns, spot size 13 mm) with the laser energy controlled at 1.0 J to obtain a gray-green WO3 ultrafine particle colloidal solution.
[0075] (4) The WO3 ultrafine particle colloidal solution from step (3) was purified by rapid rotary evaporation and then vacuum dried to obtain a black-green zero-dimensional WO3 nanoparticle powder sample.
[0076] At this energy density, the bulk WO3 material cannot be completely processed by laser and remains essentially unchanged, indicating that it is impossible to prepare ultrafine particles at low energy.
[0077] Comparative Example 2
[0078] The method for preparing WO3 nanoparticles using liquid-phase laser irradiation technology is the same as the preparation steps in Example 1, except that the laser energy is replaced by 2.2 J instead of 2.0 J, and includes the following steps:
[0079] (1) Place WO3 powder in an agate ball milling jar, add acetone for ball milling, set the ball milling speed to 400 rpm, and the ball milling time to 12 h. After drying, a light green WO3 precursor powder is obtained.
[0080] (2) Weigh 5mg of the WO3 precursor powder from step (1), measure 10mL of acetone, mix and ultrasonically disperse evenly to prepare a WO3 dispersion of 0.2mg / mL, which is yellow-green.
[0081] (3) At room temperature, the WO3 dispersion in step (2) was irradiated for 5 min using an Nd:YAG pulsed laser (pulse frequency 10 Hz, pulse width 8 ns, spot size 13 mm) with the laser energy controlled at 2.2 J to obtain a gray-green WO3 ultrafine particle colloidal solution.
[0082] (4) The WO3 ultrafine particle colloidal solution from step (3) was purified by rapid rotary evaporation and then vacuum dried to obtain a black-green zero-dimensional WO3 nanoparticle powder sample.
[0083] The results show that at this energy density, the laser reacts violently to the bulk WO3 material, which can easily cause safety hazards. At the same time, the particles grow. Therefore, the energy density range of 1.2 to 2.0 J was selected.
[0084] The technical effect is verified below using the nanoparticle samples from Examples 1-5 as examples:
[0085] Figure 1 a is an optical photograph of the WO3 dispersion. Figure 1 b is an optical photograph of the colloidal solution of WO3 ultrafine particles; in comparison, the WO3 dispersion before laser treatment is a light green colloidal solution, while after laser treatment, the colloidal solution of WO3 ultrafine particles turns black and is uniformly dispersed without precipitation, indicating that under the action of laser, the micron-sized WO3 block material is transformed into nano-sized WO3 ultrafine particles.
[0086] according to Figure 2 The transmission electron microscope (TEM) image showed that the prepared WO3 ultrafine nanoparticles (denoted as L-WO3) were spherical. The particle size distribution diagram (inset) showed that the size of the obtained WO3 ultrafine nanoparticles was about 2.84 nm, and the particle size distribution was uniform with no agglomeration.
[0087] The WO3 ultrafine nanoparticle powder sample obtained in Example 1 was redispersed in ethanol for observation (denoted as Re-L-WO3), and the results are as follows. Figure 3 As shown, the sample size was found to be around 3 nm, with uniform distribution and no agglomeration, indicating that the prepared WO3 ultrafine particles have the potential for solvent substitution.
[0088] The obtained WO3 ultrafine nanoparticles were further structurally characterized. Figure 4 The images show X-ray diffraction (XRD) patterns of WO3 samples before and after laser treatment. The laser-treated sample is L-WO3, and the untreated sample is WO3. The XRD patterns show that the diffraction peaks of WO3 correspond to the standard card (PDF#43-1035), with space group P21 / n and cell parameters [not specified]. The unit cell volume is The results confirm that WO3 is pure-phase WO3, and the high intensity of each diffraction peak indicates that WO3 has good crystallinity. After laser treatment, the diffraction peak intensity of the L-WO3 sample decreased significantly, and the (002), (020) and (200) crystal planes were observed only in the 23-24° range. The above diffraction peaks showed broadening, which indicates that laser treatment does not change the crystal structure of WO3. At the same time, the grain size of the WO3 sample after laser treatment was significantly reduced, which is consistent with the results of transmission electron microscopy.
[0089] also, Figure 5Medium-to-high resolution transmission electron microscopy images revealed distinct lattice fringes with interplanar spacing of [missing information]. Corresponding to the (202) crystal plane of WO3, it is also proven that the sample still has crystal properties after laser treatment.
[0090] A series of experimental phenomena revealed that oxides tend to form oxygen vacancies after laser treatment. The presence of vacancies plays an important role in improving their photoelectric, catalytic, and energy storage properties. Therefore, taking the zero-dimensional BiVO4 ultrafine particles prepared in Example 4 as an example, X-ray photoelectron spectroscopy (XPS) was used to characterize and analyze the elemental valence states and electronic structures of the samples before and after laser treatment. Figure 6 a represents the O1s orbitals of the BiVO4 samples before and after laser treatment. Spectral analysis revealed characteristic peaks at 530.1 eV and 532.4 eV in the initial BiVO4 sample, corresponding to lattice oxygen (O2) and crystalline oxygen (O2), respectively. L ) and adsorbed oxygen (O A L-BiVO4 ultrafine nanoparticles after laser treatment ( Figure 6 b) In addition to the two characteristic peaks mentioned above, an additional new characteristic peak appears at the position of 531.2 eV, which corresponds to the vacant oxygen (O) V This indicates that laser treatment alters the electronic structure of the BiVO4 surface, causing high-valence vanadium to gain electrons and oxygen ions to lose electrons, thus forming oxygen defects.
[0091] also, Figure 7 Further analysis of the oxygen vacancies using electron paramagnetic resonance (EPR) spectroscopy revealed that the electron spin resonance spectral signal centers of the BiVO4 samples before and after laser treatment were both located at g. iso-factor At position 2.00396, this corresponds to the signal center of the oxygen vacancy. Some oxygen vacancies also exist in the BVO precursor before laser treatment, which is due to the formation of a small number of vacancies during the precursor co-precipitation synthesis process. However, it is noteworthy that the EPR signal of the laser-treated LBVO sample is significantly enhanced, more than twice that of the precursor sample, indicating that the laser treatment process can generate more oxygen vacancies.
[0092] In summary, combining electron microscopy and X-ray characterization techniques for laser-prepared WO3 ultrafine nanoparticles, we have demonstrated the successful rapid preparation of WO3 ultrafine nanoparticles with a size less than 3 nm and uniform particle distribution using pulsed lasers. Furthermore, taking Example 4 as an example, X-ray photoelectron spectroscopy and electron paramagnetic resonance spectroscopy analysis revealed that abundant oxygen vacancy structures are easily constructed on the surface of the oxide nanoparticles during laser processing. Particularly noteworthy is that the zero-dimensional oxide nanoparticle powder prepared by this method remains unchanged and does not agglomerate after redispersing in a solvent.
[0093] After verification through similar experiments, this method has been shown to be universally applicable. A general experimental flowchart is shown below. Figure 8 As shown, the system experiments demonstrate that the laser strategy can prepare a wide variety of zero-dimensional oxide nanoparticles and can produce oxide ultrafine nanoparticle powder samples, which is beneficial for the preparation of quantum-dimensional oxide samples.
[0094] according to Figure 9 The transmission electron microscopy (TEM) images show that the prepared zero-dimensional Fe₂O₃ nanoparticles are spherical, composed of... Figure 9 The embedded particle size distribution diagram shows that the obtained zero-dimensional Fe2O3 nanoparticles are approximately 2.84 nm in size, and the particle size distribution is uniform with no agglomeration observed.
[0095] according to Figure 10 The transmission electron microscopy (TEM) image shows that the prepared zero-dimensional NiO x Nanoparticles are spherical in shape, made of Figure 10 The embedded particle size distribution diagram shows that the obtained zero-dimensional NiO x The nanoparticles are approximately 2.93 nm in size and have a uniform size distribution, with no aggregation observed.
[0096] according to Figure 11 The transmission electron microscopy (TEM) images show that the prepared zero-dimensional BiVO4 ultrafine nanoparticles are spherical, composed of... Figure 11 The embedded particle size distribution diagram shows that the obtained zero-dimensional BiVO4 nanoparticles are approximately 2.43 nm in size, and the particle size distribution is uniform with no agglomeration observed.
[0097] according to Figure 12 The transmission electron microscopy (TEM) images show that the prepared zero-dimensional LaFeO3 ultrafine nanoparticles are spherical, composed of... Figure 12 The embedded particle size distribution diagram shows that the obtained zero-dimensional LaFeO3 nanoparticles are approximately 2.93 nm in size, and the particle size distribution is uniform with no agglomeration observed.
[0098] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims and their equivalents, this invention also intends to include these modifications and variations. The above-described embodiments are merely preferred embodiments for fully illustrating the invention, and their scope of protection is not limited thereto. Equivalent substitutions or modifications made by those skilled in the art based on this invention are all within the scope of protection of this invention, which is defined by the claims.
Claims
1. A method for preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology, characterized in that, Includes the following steps: An oxide precursor with a particle size of micrometers is dispersed in a solvent, which is a non-alcoholic polar solvent, to obtain an oxide dispersion. The oxide precursor is a non-white multi-component oxide or a non-white binary oxide; The oxide dispersion was irradiated using liquid phase laser irradiation technology. The irradiation process instantly generated a high-temperature molten oxide precursor. The oxide in the high-temperature molten state condensed into nano-sized ultrafine particles in the solvent, resulting in an oxide ultrafine particle colloidal solution. The solvent in the oxide ultrafine particle colloidal solution was separated to obtain zero-dimensional oxide nanoparticles. The laser emission wavelength for irradiation treatment is 1064 nm, the laser irradiation energy is 1.2-2.0 J, and the laser irradiation range is 1.3 cm.
2. The method for preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology according to claim 1, characterized in that, The mass ratio of the oxide precursor to the volume of the solvent in the oxide dispersion is 0.2~1.5 mg / mL.
3. The method for preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology according to claim 1, characterized in that, The irradiation treatment was carried out at room temperature.
4. The method for preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology according to claim 1, characterized in that, Laser irradiation for 1-10 minutes.
5. The method for preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology according to claim 1, characterized in that, The solvent is selected from acetone, N,N'-dimethylformamide, dimethyl sulfoxide, dioxane, or ethylene glycol dimethyl ether.
6. The method for preparing zero-dimensional oxide nanoparticles using liquid-phase laser irradiation technology according to claim 1, characterized in that, The method for separating the solvent is vacuum distillation.