Cluster material and preparation method thereof
By applying an alternating field in a liquid medium to regulate cluster nucleation and growth, and combining physical and chemical methods, the problems of long cluster synthesis cycle, large size and poor uniformity in the existing technology are solved, and efficient and environmentally friendly cluster material preparation is achieved.
Patent Information
- Application Number
- CN202310755153.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-06-25
- Publication Date
- 2025-09-26
- Estimated Expiration
- 2043-06-25
AI Technical Summary
In the existing technology, chemical synthesis of clusters has the problems of long cycle and environmental pollution, while physical synthesis of clusters has large size and poor uniformity.
The metal material or alloy material is converted into metal ions, and an alternating pulse field is applied in the liquid medium. The nucleation and growth of clusters are regulated by the alternating field. By combining physical and chemical methods, small and uniform cluster materials are prepared.
It achieves the rapid acquisition of small and uniform cluster materials, improves the efficiency of chemical synthesis of clusters, and is more environmentally friendly.
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Figure CN116786835B_ABST
Abstract
Description
Technical Field
[0001] The present disclosure relates to the technical field of cluster materials, and in particular to a cluster material and a preparation method thereof. Background Art
[0002] Clusters belong to the scale concept of nanomaterials. They are a material state between atoms, molecules and bulk materials. They are microscopic aggregates composed of several or even thousands of atoms, molecules or ions through physical or chemical binding forces. As the number of atoms they contain changes, they usually have special physical and chemical properties. They have important applications in biology, medicine, energy, catalysis and other fields.
[0003] Currently, the preparation methods of cluster materials mainly include chemical methods and physical methods. Chemical methods include reducing different ions into clusters in the liquid phase through reducing agents such as sodium borohydride, thiol compounds, and reducing proteins, and adding different surfactants to modify and stabilize the clusters; physical methods include sputtering, evaporation, gas condensation, laser evaporation, thermal decomposition, etc.
[0004] The chemical method of synthesizing clusters has the problems of long cycle and environmental pollution, while the physical method of synthesizing clusters has the problems of large size and poor uniformity. Summary of the Invention
[0005] The present disclosure provides a cluster material and a preparation method thereof, so as to at least solve the above technical problems existing in the prior art.
[0006] According to a first aspect of the present disclosure, a method for preparing a cluster material is provided, the method comprising:
[0007] Convert metal materials or alloy materials into metal ions;
[0008] preparing a liquid medium, wherein the liquid medium comprises a surfactant and a solvent;
[0009] The metal ions are dispersed in the liquid medium and an alternating pulse field is applied to obtain a colloidal solution or suspension of the cluster material. The colloidal solution or suspension is centrifuged to obtain cluster material powder.
[0010] In one embodiment, the metal material or alloy material is converted into metal ions by physical methods.
[0011] In one embodiment, the method further comprises:
[0012] The metal material or alloy material is pretreated, and the pretreatment includes at least one of grinding, surface cleaning, and dispersion.
[0013] In one embodiment, the surfactant includes one of a cationic surfactant, an anionic surfactant, and a nonionic surfactant.
[0014] In one embodiment, the cationic surfactant includes one of cetyltrimethylammonium chloride, cetyltrimethylammonium bromide or dodecyldimethylbenzylammonium bromide.
[0015] In one embodiment, the anionic surfactant includes one of sodium dodecylbenzenesulfonate, sodium stearate, sodium lauryl sulfate, sodium hexadecyl sulfate, sodium lauryl polyoxyethylene ether sulfate, sodium lauryl aminoethyl sulfate, sodium diisopropylnaphthalenesulfonate, and potassium laurate.
[0016] In one embodiment, the nonionic surfactant includes one of fatty alcohol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty alcohol polyoxyethylene ether carboxylic acid, fatty acid glyceride, polysorbate, and Pluronic.
[0017] In one embodiment, the solvent includes one of water, ethanol, isopropanol, ethylene glycol, glycerol, N,N-dimethylacetamide, cyclohexane, oleic acid, and silicone oil.
[0018] In one embodiment, the alternating pulse field includes one of an electric field, a magnetic field and a laser field;
[0019] When the alternating pulse field is an electric field, the voltage range is -60-60V, the frequency is 10-50Hz, and the electric field action time is 10-60min;
[0020] When the alternating pulse field is a magnetic field, the magnetic field intensity is 0.4-1.4T, the magnetic field frequency is 10-30Hz, the duty cycle is 30%-60%, and the magnetic field action time is 10-30min;
[0021] When the alternating pulse field is a laser field, the laser wavelength is 200-1000 nm, and the laser action time is 10-30 minutes.
[0022] According to a second aspect of the present disclosure, a cluster material is provided, which is prepared according to the above method.
[0023] The present disclosure provides a cluster material and a preparation method thereof, wherein a metal material or alloy material is first converted into metal ions through different physical methods, and then the ions are dispersed in a liquid medium containing reaction raw materials, and an alternating field is applied in the liquid medium to quickly regulate the nucleation and growth of the clusters, thereby quickly obtaining a cluster material with small size and uniformity; this scheme organically combines physical and chemical methods in multiple steps, and by utilizing an alternating field to regulate the growth process of the clusters during nucleation, not only does it avoid the shortcomings of the large size and poor uniformity of clusters synthesized by the physical method, but it can also selectively select and change the reaction raw materials in the liquid medium according to the target product, thereby greatly improving the working efficiency of the chemical synthesis of clusters, and being more environmentally friendly.
[0024] It should be understood that the contents described in this section are not intended to identify the key or important features of the embodiments of the present disclosure, nor are they intended to limit the scope of the present disclosure. Other features of the present disclosure will become readily understood through the following description. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] The above and other objects, features and advantages of the exemplary embodiments of the present disclosure will become readily understood by reading the detailed description below with reference to the accompanying drawings, in which several embodiments of the present disclosure are shown by way of example and not limitation, wherein:
[0026] In the drawings, the same or corresponding reference numerals denote the same or corresponding parts.
[0027] Figure 1 A schematic flow chart of a method for preparing a cluster material according to an embodiment of the present disclosure is shown;
[0028] Figure 2 shows a TEM image of the silver clusters prepared in Example 1 of the present disclosure;
[0029] Figure 3 shows the particle size distribution of the silver clusters prepared in Example 1 of the present disclosure;
[0030] Figure 4 shows a TEM image of the copper clusters prepared in Example 2 of the present disclosure;
[0031] Figure 5 shows the particle size distribution of the copper clusters prepared in Example 2 of the present disclosure;
[0032] Figure 6 shows a TEM image of the zinc cluster prepared in Example 3 of the present disclosure;
[0033] Figure 7 shows the particle size distribution of zinc clusters prepared in Example 3 of the present disclosure;
[0034] Figure 8TEM images of the copper-zinc alloy clusters prepared in Example 4 of the present disclosure are shown;
[0035] Figure 9 shows the particle size distribution of the copper-zinc alloy clusters prepared in Example 4 of the present disclosure;
[0036] Figure 10 shows a TEM image of the copper-titanium alloy cluster prepared in Example 5 of the present disclosure;
[0037] Figure 11 shows the particle size distribution of the copper-titanium alloy clusters prepared in Example 5 of the present disclosure;
[0038] Figure 12 TEM images of zinc-titanium alloy clusters prepared in Example 6 of the present disclosure are shown;
[0039] Figure 13 TEM images of zinc-titanium alloy clusters prepared in Example 6 of the present disclosure are shown;
[0040] Figure 14 shows the particle size distribution of the zinc-titanium alloy clusters prepared in Example 6 of the present disclosure;
[0041] Figure 15 shows a TEM image of the cobalt oxide clusters prepared in Example 7 of the present disclosure;
[0042] Figure 16 shows a TEM image of the cobalt oxide clusters prepared in Example 7 of the present disclosure;
[0043] Figure 17 shows the particle size distribution of the cobalt oxide clusters prepared in Example 7 of the present disclosure;
[0044] Figure 18 shows a TEM image of the nickel sulfide cluster prepared in Example 8 of the present disclosure;
[0045] Figure 19 shows the particle size distribution of nickel sulfide clusters prepared in Example 8 of the present disclosure;
[0046] Figure 20 shows a TEM image of the iron hydroxide clusters prepared in Example 9 of the present disclosure;
[0047] Figure 21 The particle size distribution diagram of the iron hydroxide clusters prepared in Example 9 of the present disclosure is shown. DETAILED DESCRIPTION
[0048] To make the purposes, features, and advantages of the present disclosure more apparent and understandable, the technical solutions in the embodiments of the present disclosure will be clearly and completely described below in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present disclosure, not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of the present disclosure without creative work shall fall within the scope of protection of the present disclosure.
[0049] like Figure 1 The figure shows a schematic flow diagram of a method for preparing a cluster material, which includes:
[0050] S1. Converting metal materials or alloy materials into metal ions;
[0051] The metal material or alloy material can be a block material or a powder material, and the present invention does not limit the state of the metal material or alloy material.
[0052] In one embodiment, before converting the metal material or alloy material into metal ions, the method further includes: pre-treating the metal material or alloy material, wherein the pre-treatment includes grinding and surface cleaning of bulk material or cleaning and dispersion of powder material.
[0053] The pretreated metal material or alloy material is then placed in a sealed or semi-open sample chamber, where the sample chamber environment can be vacuum, atmospheric air, gases of varying compositions, or liquids. The metal material or alloy material is then converted into metal ions using a physical method, including but not limited to a laser beam, electron beam, ion beam, electric arc, and the like.
[0054] S2. preparing a liquid medium, wherein the liquid medium comprises a surfactant and a solvent;
[0055] Surfactants include cationic surfactants such as cetyltrimethylammonium chloride, cetyltrimethylammonium bromide, or dodecyldimethylbenzylammonium bromide; anionic surfactants such as sodium dodecylbenzenesulfonate, sodium stearate, sodium lauryl sulfate, sodium cetyl sulfate, sodium lauryl alcohol polyoxyethylene ether sulfate, sodium lauryl aminoethyl sulfate, sodium diisopropylnaphthalenesulfonate, and potassium laurate; and nonionic surfactants such as fatty alcohol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty alcohol polyoxyethylene ether carboxylic acid, fatty acid glycerides, polysorbate, and pluronic.
[0056] Solvents include water, ethanol, isopropanol, ethylene glycol, glycerol, N,N-dimethylacetamide, cyclohexane, oleic acid, and silicone oil.
[0057] S3. Dispersing the metal ions in the liquid medium and applying an alternating pulse field. Under the action of the alternating pulse field and the surfactant, the metal ions react to form clusters, thereby obtaining a colloidal solution or suspension of the cluster material. After centrifuging the colloidal solution or suspension, a cluster material powder can be obtained.
[0058] The metal ions prepared in step S1 are dispersed into the liquid medium of step S2, and the dispersion mode includes air flow or liquid flow. An alternating pulse field is further applied to induce and control the generation reaction and material dispersion of the material to obtain a cluster material with a scale below 5nm. The alternating pulse field includes an electric field, a magnetic field or a laser field to obtain a solution or suspension of the cluster material, and the solution or suspension is subjected to high-speed centrifugation to obtain a cluster material powder. The cluster material finally prepared includes metal clusters, alloy clusters, and various compound clusters, such as metal oxide clusters, metal sulfide clusters, and hydroxide clusters.
[0059] When the alternating pulse field is an electric field, the voltage range is -60-60V, the frequency is 10-50Hz, and the electric field action time is 10-60min;
[0060] When the alternating pulse field is a magnetic field, the magnetic field intensity is 0.4-1.4T, the magnetic field frequency is 10-30Hz, the duty cycle is 30%-60%, and the magnetic field action time is 10-30min;
[0061] When the alternating pulse field is a laser field, the laser wavelength is 200-1000 nm, and the laser action time is 10-30 minutes.
[0062] The present invention combines physical and chemical methods in a multi-step organic composite. By utilizing an alternating field to regulate the growth process of cluster nucleation during cluster nucleation, it not only avoids the disadvantages of large size and poor uniformity of clusters synthesized by the physical method, but also allows for targeted selection and change of reaction raw materials in a liquid medium according to the target product, thereby greatly improving the working efficiency of chemical cluster synthesis and being more environmentally friendly.
[0063] The technical solution of the present invention is further described in detail below with reference to specific embodiments.
[0064] Example 1
[0065] A method for preparing a cluster material, wherein the cluster material is a silver cluster, comprises the following steps:
[0066] S11. Polish a silver sheet measuring 100 mm × 100 mm × 5 mm to remove surface impurities, then clean the surface by ultrasonic treatment with ethanol and deionized water, respectively. Place the treated silver sheet in a sealed sample chamber, introduce a mixture of argon and oxygen in a ratio of 95%:5%, and then bombard the silver sheet with a high-energy ion beam for 5 minutes to generate silver atoms. The silver atoms, under the action of oxygen, generate a large amount of silver ions.
[0067] S12, dissolving 200 mg of a cationic surfactant, dodecyldimethylbenzylammonium bromide, in 5 L of deionized water and stirring magnetically for 10 minutes to obtain a uniform and transparent liquid medium;
[0068] S13: The silver ions obtained in the above-mentioned S11 sample cavity are introduced into the container of S12 liquid medium by air flow, and the silver ions are fully dispersed in the aqueous solution of dodecyldimethylbenzylammonium bromide by magnetic stirring. The nucleation and growth of silver clusters are controlled by adding a pulsed laser irradiation above the liquid surface. The wavelength of the pulsed laser is 254nm, and the laser action time is 10 minutes. The test found that the concentration of silver clusters is 400ppm.
[0069] The micromorphology and particle size distribution of the prepared silver clusters were characterized and analyzed. The morphology of the prepared silver clusters was observed by transmission electron microscopy (TEM). The TEM images are as follows: Figure 2 The particle size distribution of the prepared silver clusters is shown in Figure 3 As shown. Figure 2-3 It can be seen that according to the preparation method of Example 1, a silver cluster material with a diameter of about 0.7 nm can be obtained.
[0070] Example 2
[0071] A method for preparing a cluster material, wherein the cluster material is a copper cluster, comprises the following steps:
[0072] S21. Polish a copper sheet measuring 100 mm × 100 mm × 5 mm to remove surface impurities, then clean the surface by ultrasonic treatment with ethanol and deionized water, respectively. Place the treated silver sheet in a sealed sample chamber, and introduce a mixture of argon and oxygen into the chamber at a ratio of 95%:5%. Then, bombard the copper sheet with a high-energy ion beam for 5 minutes to generate copper atoms, which, under the action of oxygen, generate a large amount of copper ions.
[0073] S22, dissolving 500 mg of anionic surfactant sodium lauryl sulfate in 5 L of deionized water and stirring magnetically for 10 minutes to obtain a uniform and transparent liquid medium;
[0074] S23: The copper ions obtained in the above-mentioned S21 sample cavity are introduced into the container of S22 liquid medium by air flow, and the copper ions are fully dispersed in the aqueous solution of sodium dodecyl sulfate by magnetic stirring. A pulsed laser is added above the liquid surface to control the nucleation and growth of copper clusters. The wavelength of the pulsed laser is 532nm, and the laser action time is 20 minutes. The test found that the concentration of copper clusters was 1000ppm.
[0075] The micromorphology and particle size distribution of the prepared copper clusters were characterized and analyzed. The morphology of the prepared copper clusters was observed by transmission electron microscopy (TEM). The TEM images are as follows: Figure 4 The particle size distribution of the prepared copper clusters is shown in Figure 5 As shown. Figure 4-5 The TEM image and particle size distribution results show that according to the preparation method of Example 2, a copper cluster material with a diameter of about 2 nm can be obtained.
[0076] Example 3
[0077] A method for preparing a cluster material, wherein the cluster material is a zinc cluster, comprises the following steps:
[0078] S31. A zinc sheet measuring 100 mm × 100 mm × 5 mm was polished to remove surface impurities, and then the surface was cleaned by ultrasonic treatment with ethanol and deionized water, respectively. The treated zinc sheet was placed in a sealed sample chamber, and a mixture of argon and oxygen was introduced into the sample chamber, with the ratio of argon to oxygen being 95%:5%. The zinc sheet was then bombarded with a high-energy ion beam for 5 minutes to generate zinc atoms. The zinc atoms, under the action of oxygen, produced a large amount of zinc ions.
[0079] S32, dissolving 1000 mg of a nonionic surfactant, sodium stearate, in 5 L of deionized water and stirring magnetically for 10 minutes to obtain a uniform and transparent liquid medium;
[0080] S33: The zinc ions obtained in the above-mentioned S31 sample cavity are introduced into the container of S32 liquid medium by air flow, and the zinc ions are fully dispersed in the aqueous solution of sodium stearate by magnetic stirring. A pulsed laser is added above the liquid surface to control the nucleation and growth of zinc clusters. The wavelength of the pulsed laser is 1064nm, and the laser action time is 30 minutes. The test found that the concentration of zinc clusters was 2500ppm.
[0081] The micromorphology and particle size distribution of the prepared zinc clusters were characterized and analyzed. The morphology of the prepared zinc clusters was observed by transmission electron microscopy (TEM). The TEM images are as follows: Figure 6 The particle size distribution of zinc clusters is shown in Figure 7The results of TEM images and particle size distribution diagrams show that according to the preparation method of Example 3, zinc cluster materials with a diameter of about 3.5 nm can be obtained.
[0082] Example 4
[0083] A method for preparing a cluster material, wherein the cluster material is a copper-zinc alloy cluster, comprises the following steps:
[0084] S41: A copper-zinc alloy target (copper: zinc = 80%: 20%) with a diameter of 50 mm and a thickness of 5 mm was polished to remove the surface oxide layer. The surface oil was removed by ultrasonic cleaning in cyclohexane. The alloy target was then ultrasonically cleaned in ethanol. The treated copper-zinc alloy target was then placed in a sealed sample chamber. The sample chamber environment was vacuumed to a vacuum degree of 1.0×10 - 3 Pa, using electron beam bombardment of copper-zinc alloy target to produce copper-zinc metal ions;
[0085] S42: 200 mg of surfactant cetyltrimethylammonium bromide was added to 2 L of N,N-dimethylacetamide and magnetically stirred for 10 minutes to form a uniform liquid medium;
[0086] S43: The copper-zinc ions obtained in the sample cavity of S41 are dispersed into a container containing the liquid medium described in S42 by air flow, and the copper-zinc ions are fully dispersed in the N,N-dimethylacetamide solution of hexadecyltrimethylammonium bromide by magnetic stirring. At the same time, a pulsed electric field is added to the side of the liquid container to control the nucleation and growth of copper-zinc alloy clusters. The pulsed electric field is a triangular wave with a duty cycle of 50%, a voltage range of -30-30V, a frequency of 10Hz, and an electric field action time of 10 minutes.
[0087] The micromorphology and particle size distribution of the prepared copper-zinc clusters were characterized and analyzed. The morphology of the prepared copper-zinc clusters was observed by transmission electron microscopy (TEM). The TEM images are shown in Figure 2. Figure 8 As shown; particle size distribution is as Figure 9 The results of TEM images and particle size distribution diagrams show that according to the preparation method of Example 4, a copper-zinc cluster material with a diameter of about 2 nm can be obtained.
[0088] Example 5
[0089] A method for preparing a cluster material, wherein the cluster material is a copper-titanium alloy cluster, comprises the following steps:
[0090] S51: A copper-titanium alloy target (copper: titanium = 80%: 20%) with a diameter of 50 mm and a thickness of 5 mm was polished to remove the surface oxide layer. The surface oil was removed by ultrasonic cleaning in cyclohexane. The alloy target was then ultrasonically cleaned in ethanol. The treated copper-titanium alloy target was then placed in a sealed sample chamber. The sample chamber environment was vacuumed to a vacuum degree of 1.0×10 - 3 Pa, using electron beam to bombard copper-titanium alloy target to produce copper-titanium metal ions;
[0091] S52: 200 mg of surfactant cetyltrimethylammonium bromide was added to 2 L of ethylene glycol and magnetically stirred for 10 minutes to form a uniform liquid medium;
[0092] S53: The copper-titanium ions obtained in the above-mentioned S51 sample cavity are dispersed into a container containing the liquid medium described in S52 by air flow, and the copper-titanium ions are fully dispersed in the ethylene glycol solution of hexadecyltrimethylammonium bromide by magnetic stirring. At the same time, a pulsed electric field is added to the side of the liquid container to control the nucleation and growth of copper-titanium alloy clusters. The pulsed electric field is a square wave with a duty cycle of 40%, a voltage range of -40-40V, a frequency of 30Hz, and an electric field action time of 20 minutes.
[0093] The micromorphology and particle size distribution of the prepared copper-titanium clusters were characterized and analyzed. The TEM images of the prepared copper-titanium clusters are shown in Figure 2. Figure 10 As shown; particle size distribution is as Figure 11 The results of TEM images and particle size distribution diagrams show that according to the preparation method of Example 5, a copper-titanium cluster material with a diameter of about 2 nm can be obtained.
[0094] Example 6
[0095] A method for preparing a cluster material, wherein the cluster material is a zinc-titanium alloy cluster, comprises the following steps:
[0096] S61: A zinc-titanium alloy target (zinc:titanium = 80%:20%) with a diameter of 50 mm and a thickness of 5 mm was polished to remove the surface oxide layer. The surface oil was removed by ultrasonic cleaning in cyclohexane. The alloy target was then ultrasonically cleaned in ethanol. The treated zinc-titanium alloy target was then placed in a sealed sample chamber. The sample chamber environment was vacuumed to a vacuum degree of 1.0×10 - 3 Pa, uses electron beam to bombard zinc-titanium alloy target to produce zinc-titanium metal ions;
[0097] S62: 200 mg of surfactant cetyltrimethylammonium bromide was added to 2 L of glycerol and magnetically stirred for 10 minutes to form a uniform liquid medium;
[0098] S63: The zinc-titanium ions obtained in the above-mentioned S61 sample cavity are dispersed into a container containing the liquid medium described in S62 by air flow, and the zinc-titanium ions are fully dispersed in the propylene glycol solution of hexadecyltrimethylammonium bromide by magnetic stirring. At the same time, a pulsed electric field is added to the side of the liquid container to control the nucleation and growth of zinc-titanium alloy clusters. The pulsed electric field is a sawtooth wave with a duty cycle of 20%, a voltage range of -60-60V, a frequency of 50Hz, and an electric field action time of 30 minutes.
[0099] The microstructure and particle size distribution of the prepared zinc-titanium clusters were characterized and analyzed. The TEM images of the prepared zinc-titanium clusters are shown in Figure 2. Figure 12 and 13 As shown; particle size distribution is as Figure 14 The results of TEM images and particle size distribution diagrams show that according to the preparation method of Example 6, zinc-titanium cluster materials with a diameter of about 2.6 nm can be obtained.
[0100] Example 7
[0101] A method for preparing a cluster material, wherein the cluster material is a cobalt oxide cluster, comprises the following steps:
[0102] S71: 5 g of metallic cobalt powder is placed in an alumina crucible, and then 100 mL of octadecene is added to the crucible. The crucible containing the metallic cobalt powder and octadecene is placed in a semi-open sample chamber, and the cobalt powder in the octadecene is irradiated with a laser beam to produce a cobalt ion solution;
[0103] S72: Dispersing 1000 mg of the surfactant sodium lauryl polyoxyethylene ether sulfate in 10 L of deionized water, and ultrasonically dispersing the mixture to form a uniform liquid medium;
[0104] S73: The cobalt ions obtained in the sample chamber in S71 are dispersed into a container containing the liquid medium described in S72 using a liquid flow. Circulation is performed to fully disperse the cobalt ions in the aqueous solution containing sodium lauryl polyoxyethylene ether sulfate. Simultaneously, a pulsed magnetic field is applied to the side of the liquid container to control the nucleation and growth of cobalt oxide clusters. The magnetic field intensity is 0.4 T, the frequency is 10 Hz, the duty cycle is 60%, and the magnetic field application time is 10 minutes.
[0105] The micromorphology and particle size distribution of the prepared cobalt oxide clusters were characterized and analyzed. The TEM images of the cobalt oxide clusters are shown in Figure 2. Figure 15-16 As shown; particle size distribution is as Figure 17 The results of TEM images and particle size distribution diagrams show that according to the preparation method of Example 7, a cobalt oxide cluster material with a diameter of about 2.6 nm can be obtained.
[0106] Example 8
[0107] A method for preparing a cluster material, wherein the cluster material is a nickel sulfide cluster, comprises the following steps:
[0108] S81: 5 g of metallic nickel powder is placed in an alumina crucible, and then 100 mL of octadecene is added to the crucible. The crucible containing the metallic nickel powder and octadecene is placed in a semi-open sample chamber, and the nickel powder in the octadecene is irradiated with a laser beam to produce a nickel ion solution;
[0109] S82: dispersing 1000 mg of a surfactant, polyvinyl pyrrolidone, in 10 L of deionized water, and then adding 1000 mg of a sulfur source, methionine, and ultrasonically dispersing the mixture to form a uniform liquid medium;
[0110] S83: The nickel ions obtained in the sample chamber of S81 are dispersed into a container containing the liquid medium described in S82 using a liquid flow. Circulating the nickel ions allows the nickel ions to be fully dispersed in the aqueous solution containing polyvinyl pyrrolidone. Simultaneously, a pulsed magnetic field is applied to the side of the liquid container to control the nucleation and growth of nickel sulfide clusters. The magnetic field intensity is 1.0 T, the frequency is 20 Hz, the duty cycle is 40%, and the magnetic field is applied for 20 minutes.
[0111] The micromorphology and particle size distribution of the prepared nickel sulfide clusters were characterized and analyzed. The TEM images of the nickel sulfide clusters are shown in Figure 2. Figure 18 As shown; particle size distribution is as Figure 19 The results of TEM images and particle size distribution diagrams show that according to the preparation method of Example 8, nickel sulfide cluster materials with a diameter of about 2.5 nm can be obtained.
[0112] Example 9
[0113] A method for preparing a cluster material, wherein the cluster material is an iron hydroxide cluster, comprises the following steps:
[0114] S81: 5 g of metallic iron powder is placed in an alumina crucible, and then 100 mL of octadecene is added to the crucible. The crucible containing the metallic iron powder and octadecene is placed in a semi-open sample chamber, and the iron powder in the octadecene is irradiated with a laser beam to produce an iron ion solution;
[0115] S82: 1000 mg of the surfactant Pluronic was dispersed in 10 L of deionized water, and 100 mg of sodium hydroxide was added and ultrasonically dispersed to form a uniform liquid medium;
[0116] S83: The iron ions obtained in the sample chamber in S81 are dispersed using liquid flow into a container containing the liquid medium described in S82. A circulating flow is used to fully disperse the iron ions in the aqueous solution containing pluronic and sodium hydroxide. Simultaneously, a pulsed magnetic field is applied to the side of the liquid container to control the nucleation and growth of iron hydroxide clusters. The magnetic field intensity is 1.4 T, the frequency is 30 Hz, the duty cycle is 30%, and the magnetic field is applied for 30 minutes.
[0117] The microstructure and particle size distribution of the prepared iron hydroxide clusters were characterized and analyzed. The TEM images of the iron hydroxide clusters are shown in Figure 2. Figure 20 As shown; particle size distribution is as Figure 21 The TEM image and particle size distribution results show that according to the preparation method of Example 9, an iron hydroxide cluster material with a diameter of about 2.3 nm can be obtained.
[0118] It should be understood that the various forms of the processes shown above can be used to reorder, add, or delete steps. For example, the steps described in this disclosure can be performed in parallel, sequentially, or in a different order, as long as the desired results of the technical solutions of this disclosure can be achieved, and this document is not limited here.
[0119] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features being referred to. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. Throughout the present disclosure, "plurality" means two or more, unless otherwise specifically defined.
[0120] The above description is merely a specific embodiment of the present disclosure, but the scope of protection of the present disclosure is not limited thereto. Any changes or substitutions that can be easily conceived by a person skilled in the art within the technical scope disclosed in this disclosure should be included in the scope of protection of the present disclosure. Therefore, the scope of protection of the present disclosure should be based on the scope of protection of the claims.
Claims
1. A method for preparing a cluster material, characterized in that: The method comprises: Convert metal materials or alloy materials into metal ions; preparing a liquid medium, wherein the liquid medium comprises a surfactant and a solvent; The metal ions are dispersed in the liquid medium and an alternating pulse field is applied to obtain a colloidal solution or suspension of the cluster material; the colloidal solution or suspension is centrifuged to obtain a cluster material powder; The alternating pulse field includes one of an electric field, a magnetic field and a laser field; When the alternating pulse field is an electric field, the voltage range is -60-60V, the frequency is 10-50Hz, and the electric field action time is 10-60min; When the alternating pulse field is a magnetic field, the magnetic field intensity is 0.4-1.4T, the magnetic field frequency is 10-30Hz, the duty cycle is 30%-60%, and the magnetic field action time is 10-30min; When the alternating pulse field is a laser field, the laser wavelength is 200-1000 nm, and the laser action time is 10-30 minutes.
2. The method according to claim 1, characterized in that The metal material or alloy material is converted into metal ions by a physical method.
3. The method according to claim 1, characterized in that The method further includes: The metal material or alloy material is pretreated, and the pretreatment includes at least one of grinding, surface cleaning, and dispersion.
4. The method according to claim 1, wherein The surfactant includes one of a cationic surfactant, an anionic surfactant and a nonionic surfactant.
5. The method according to claim 4, characterized in that The cationic surfactant includes one of cetyltrimethylammonium chloride, cetyltrimethylammonium bromide or dodecyldimethylbenzylammonium bromide.
6. The method according to claim 4, characterized in that The anionic surfactant includes one of sodium dodecylbenzenesulfonate, sodium stearate, sodium lauryl sulfate, sodium hexadecyl sulfate, sodium lauryl polyoxyethylene ether sulfate, sodium lauryl aminoethyl sulfate, sodium diisopropylnaphthalenesulfonate, and potassium laurate.
7. The method according to claim 4, characterized in that The nonionic surfactant includes one of fatty alcohol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty alcohol polyoxyethylene ether carboxylic acid, fatty acid glyceride, polysorbate, and Pluronic.
8. The method according to claim 1, characterized in that The solvent includes one of water, ethanol, isopropanol, ethylene glycol, glycerol, N,N-dimethylacetamide, cyclohexane, oleic acid, and silicone oil.
9. A cluster material, characterized in that Prepared according to the method according to any one of claims 1 to 8.
Citation Information
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