CN112658275A - Method for preparing ruthenium-iridium nano alloy by using laser irradiation acoustic suspension liquid drop - Google Patents
Method for preparing ruthenium-iridium nano alloy by using laser irradiation acoustic suspension liquid drop Download PDFInfo
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Abstract
The invention discloses a method for preparing ruthenium-iridium nano alloy by using laser irradiation acoustic suspension liquid drops, which comprises the following steps: dissolving ruthenium salt, iridium salt and polyvinylpyrrolidone in ethylene glycol, then carrying out acoustic suspension treatment to obtain suspension liquid drops, and carrying out laser irradiation treatment on the suspension liquid drops to prepare the ruthenium-iridium nano alloy. The method is simple and convenient to operate, and opens up a new way for trace, quick, controllable and low-energy-consumption preparation of the ruthenium-iridium nano alloy.
Description
Technical Field
The invention relates to a method for preparing ruthenium-iridium nano alloy by using laser irradiation acoustic suspension liquid drops, belonging to the technical field of novel preparation of noble metal nano materials.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The metal nanoparticles have wide application prospects in the fields of catalysis (CN 111185220A), sensing (CN 111398396A), optics (CN 111253936A), medicine and biological engineering (CN 111420057A) and the like due to unique size effect, surface effect and electronic state. Because each metal element has a unique electronic arrangement state, alloying can obtain an electronic structure different from that of a single metal element, and further influences the performance of the metal element in different applications. Numerous studies have shown that the main factors affecting the properties of nanoalloys are the size of the alloy (J Am ChemSoc, 2014, 136 (19): 6978), the elemental composition ratio (J Am ChemSoc, 2017, 139 (13): 4643) and the internal composition distribution (Nat Chem, 2014, 6 (4): 320). Therefore, developing a new preparation technology to realize accurate size control, arbitrary composition of components and controllable component distribution of the nano alloy has significant scientific significance and engineering value.
Ruthenium is a polyvalent rare metal element. It has the characteristics of stable property, strong corrosion resistance, high hardness and excellent electrical and catalytic performances, and is often used for manufacturing hard alloys and electric contact alloys and used as a catalyst for hydrogenation, oxidation, isomerization and reforming reactions (CN 111500914A). Iridium is a rare noble metal material, is considered to be the most corrosion-resistant metal element, has excellent thermal stability, and is widely used for manufacturing crucibles for high-temperature reactions, scientific instruments, thermocouples, resistance wires, and the like. Like other platinum group metal alloys, iridium alloys strongly adsorb organics and are useful as catalyst materials (CN 111389395 a). Ruthenium and iridium have high intersolubility, the components of the ruthenium-iridium alloy are continuously adjustable in a large range, and the advantages of ruthenium and iridium can be complemented by preparing the ruthenium and iridium into the alloy. Ruthenium iridium alloys have been used as high temperature thermocouple materials, catalysts, anti-tumor materials, and luminescent materials.
The ruthenium-iridium nano alloy has unique performance different from that of a bulk alloy material, and the realization of the controllable preparation of the ruthenium-iridium nano alloy is an effective means for widening the performance and the application of the ruthenium-iridium nano alloy. According to the research of the inventor, the widely adopted nano alloy preparation method relates to the reaction on a container or a substrate, heterogeneous nucleation is easy to occur, the composition segregation and the size are not controllable, and finally the physicochemical property of the nano alloy is unstable. Therefore, the development of a nano alloy preparation method for realizing accurate size control, arbitrary composition of components and controllable component distribution of the material is urgently needed.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide a method for preparing ruthenium-iridium nano alloy by utilizing laser irradiation acoustic suspension liquid drops, which can realize the container-free reaction to form ultra-small particles and mutual dissolution of elements, and overcome the agglomeration and particle growth caused by heterogeneous nucleation; avoiding component segregation in the reaction process to form homogeneous alloy; the metal reduction temperature is instantly reached, and the synchronous reduction of different types of metal ions is realized to form a solid solution structure; micro local oscillation and micro reaction are realized, and the waste of raw materials and energy caused by reaction in the traditional container is overcome; breaking through the entropy limit and obtaining multi-component metastable alloy; the alloy components and the component distribution are continuously adjustable.
In order to achieve the purpose, the technical scheme of the invention is as follows:
on the one hand, the method for preparing the ruthenium-iridium nano alloy by using laser irradiation acoustic suspension liquid drops comprises the steps of dissolving ruthenium salt, iridium salt and polyvinylpyrrolidone in ethylene glycol, then carrying out acoustic suspension treatment to obtain suspension liquid drops, and carrying out laser irradiation treatment on the suspension liquid drops to prepare the ruthenium-iridium nano alloy.
The method can carry out the reaction process under the condition of no container by utilizing acoustic suspension, and simultaneously cooperates with laser irradiation, so that the rapid synchronous reduction of the ruthenium and iridium metal ions by the glycol can be realized, and the generation of heterogeneous nucleation is avoided.
On the other hand, the ruthenium-iridium nano alloy is prepared by the method.
The invention has the beneficial effects that:
the method can realize the reduction of ruthenium and iridium metal ions by ethylene glycol within 60s to generate the ruthenium-iridium nano alloy with uniform granularity, adjustable components and granularity and good dispersibility, the granularity of the prepared ruthenium-iridium nano alloy is continuously adjustable within the range of 2-100 nm, and the molar ratio of ruthenium to iridium is 20: 1-1: the range of 20 is continuously adjustable, and the distribution of the components is uniform and controllable. The invention can open up a new way for the simple, convenient, rapid, low-energy-consumption and controllable preparation of the nano alloy and powerfully promote the development of the related field of the high-performance nano alloy.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a transmission electron microscope image of a ruthenium iridium nano alloy prepared in example 1;
FIG. 2 is a transmission electron microscope image of a ruthenium iridium nano alloy prepared in example 2;
FIG. 3 is a transmission electron microscope image of Ru-Ir nanoalloy prepared in example 3;
FIG. 4 is a transmission electron microscope image of Ru-Ir nanoalloy prepared in example 4;
FIG. 5 is a transmission electron microscope image of the Ru-Ir nanoalloy prepared in example 5.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In view of the defects of easy generation of heterogeneous nucleation, component segregation, uncontrollable size, long preparation time and the like of the existing method for preparing the ruthenium-iridium nano alloy, the invention provides a method for preparing the ruthenium-iridium nano alloy by utilizing laser irradiation acoustic suspension liquid drops.
The invention provides a method for preparing ruthenium-iridium nano alloy by using laser irradiation acoustic suspension liquid drops, which comprises the steps of dissolving ruthenium salt, iridium salt and polyvinylpyrrolidone in ethylene glycol, then carrying out acoustic suspension treatment to obtain suspension liquid drops, and carrying out laser irradiation treatment on the suspension liquid drops to prepare the ruthenium-iridium nano alloy.
The method can carry out the reaction process under the condition of no container by utilizing acoustic suspension, and simultaneously cooperates with laser irradiation, so that the rapid synchronous reduction of the ruthenium and iridium metal ions by the glycol can be realized, and the generation of heterogeneous nucleation is avoided.
The ruthenium salt according to the present invention means a compound having a cation of ruthenium ion, for example, ruthenium acetate.
The iridium salt in the present invention refers to a compound in which the cation is an iridium ion, for example, iridium acetate.
In some examples of this embodiment, the molar ratio of ruthenium salt to iridium salt is 0.05 to 20: 1.
In some examples of this embodiment, the concentration of the ruthenium salt is 5 to 100mmol/L and the concentration of the iridium salt is 5 to 100mmol/L in the reaction system.
In some examples of this embodiment, the concentration of polyvinylpyrrolidone in the reaction system is 0.1 to 50 g/L.
In some embodiments of this embodiment, the suspended liquid droplet has a volume of 1 to 200. mu.L.
In some examples of this embodiment, the output power of the laser is 10-80W during the laser irradiation treatment.
In some examples of this embodiment, the laser irradiation treatment time is 5 to 60 seconds.
In order to obtain purer ruthenium-iridium nano-alloy, some examples of the embodiment provide a pure method in which the suspension liquid after laser irradiation treatment is subjected to centrifugal purification treatment.
In one or more embodiments, in the centrifugal purification treatment, the centrifugal rotation speed is 10000-13000 rpm, and the centrifugal time is 20-60 min.
In one or more embodiments, the number of centrifugal purification treatments is 3-6.
In one or more embodiments, the solvent used in the centrifugal purification process is methanol, ethanol, propanol, isopropanol, or water.
In one or more embodiments, the centrifugal purification process is followed by drying. The drying conditions were: vacuum drying at 55-65 ℃ for 1-3 h.
In another embodiment of the invention, the ruthenium-iridium nano alloy is prepared by the method.
In one or more embodiments of this embodiment, the force is 2 to 100 nm.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1:
dissolving 25 mu mol of ruthenium acetate, 25 mu mol of iridium acetate and 0.5mg of polyvinylpyrrolidone in 5mL of glycol by ultrasonic wave to obtain a solution; extracting 35 mu L of the solution by using a syringe, and transferring the solution to a single-axis acoustic suspension automatic tuning device to obtain a suspension drop; irradiating the suspension drop for 10s by using a laser, wherein the ethylene glycol performs a reduction reaction on ruthenium ions and iridium ions, and the output power of the laser is 50W; collecting the suspension after reaction into a centrifuge tube with the volume of 1.5mL, adding methanol until the total volume of the liquid is 1mL, and performing centrifugal purification for 6 times in a centrifuge at the rotation speed of 13000rmp to obtain a solid product, wherein the centrifugation time is 60min each time; and transferring the solid product after centrifugal purification to a vacuum drying oven to dry for 2h at the temperature of 60 ℃ to obtain the black ruthenium-iridium nano alloy.
As can be seen from the transmission electron microscope image in FIG. 1, the Ru-Ir nano alloy prepared by the embodiment has uniform particle size distribution of about 2nm, good particle dispersibility and no obvious agglomeration phenomenon.
Example 2:
dissolving 25 mu mol of ruthenium acetate, 500 mu mol of iridium acetate and 0.1g of polyvinylpyrrolidone into 5mL of glycol by ultrasonic wave to obtain a solution; extracting 35 mu L of the solution by using a syringe, and transferring the solution to a single-axis acoustic suspension automatic tuning device to obtain a suspension drop; irradiating the suspension drop by a laser for 10s, wherein the ethylene glycol performs reduction reaction on ruthenium ions and iridium ions, and the output power of the laser is 40W; collecting the suspension after reaction into a centrifuge tube with the volume of 1.5mL, adding ethanol until the total volume of the liquid is 1mL, and centrifuging and purifying for 5 times in a centrifuge at the rotating speed of 12000rmp to obtain a solid product, wherein the centrifugation time is 40min each time; and transferring the solid product after centrifugal purification to a vacuum drying oven to dry for 2h at the temperature of 60 ℃ to obtain the black ruthenium-iridium nano alloy.
The transmission electron microscope image of fig. 2 shows that the ruthenium-iridium nano alloy prepared by the embodiment has uniform particle size distribution of about 3-5 nm, good particle dispersibility and no agglomeration phenomenon.
Example 3:
dissolving 500 mu mol of ruthenium acetate, 25 mu mol of iridium acetate and 0.2g of polyvinylpyrrolidone into 5mL of glycol by ultrasonic wave to obtain a solution; extracting 20 mu L of the solution by using a syringe, and transferring the solution to a single-axis acoustic suspension automatic tuning device to obtain a suspension drop; irradiating the suspension drop for 30s by using a laser, wherein the ethylene glycol performs a reduction reaction on ruthenium ions and iridium ions, and the output power of the laser is 25W; collecting the suspension after reaction into a centrifugal tube with the volume of 1.5mL, adding propanol until the total volume of the liquid is 1mL, and carrying out centrifugal purification for 4 times in a centrifugal machine at the rotating speed of 11000rmp to obtain a solid product, wherein the centrifugal time is 50min each time; and transferring the solid product after centrifugal purification to a vacuum drying oven to dry for 2h at the temperature of 60 ℃ to obtain the black ruthenium-iridium nano alloy.
The transmission electron microscope image of fig. 3 shows that the ruthenium-iridium nano alloy prepared by the embodiment has uniform particle size distribution of about 8-10 nm, good particle dispersibility and no agglomeration phenomenon.
Example 4:
dissolving 150 mu mol of ruthenium acetate, 40 mu mol of iridium acetate and 0.125g of polyvinylpyrrolidone into 5mL of glycol by ultrasonic wave to obtain a solution; extracting 25 mu L of the solution by using a syringe, and transferring the solution to a single-axis acoustic suspension automatic tuning device to obtain a suspension drop; irradiating the suspension drop for 15s by using a laser, wherein the ethylene glycol performs a reduction reaction on ruthenium ions and iridium ions, and the output power of the laser is 35W; collecting the suspension after reaction into a centrifuge tube with the volume of 1.5mL, adding methanol until the total volume of the liquid is 1mL, and centrifuging and purifying for 5 times in a centrifuge at the rotating speed of 11500rmp to obtain a solid product, wherein the centrifugation time is 25min each time; and transferring the solid product after centrifugal purification to a vacuum drying oven to dry for 2h at the temperature of 60 ℃ to obtain the black ruthenium-iridium nano alloy.
The transmission electron microscope image of fig. 4 shows that the ruthenium-iridium nano alloy prepared by the embodiment has uniform particle size distribution of about 12-15 nm, good particle dispersibility and no agglomeration phenomenon.
Example 5:
dissolving 500 mu mol of ruthenium acetate, 500 mu mol of iridium acetate and 0.25g of polyvinylpyrrolidone in 5mL of glycol by ultrasonic wave to obtain a solution; pumping 200 mu L of the solution by using a syringe, and transferring the solution to a single-axis acoustic suspension automatic tuning device to obtain a suspension drop; irradiating the suspension drop for 60s by using a laser, wherein the ethylene glycol performs a reduction reaction on ruthenium ions and iridium ions, and the output power of the laser is 20W; collecting the suspension after reaction into a centrifuge tube with the volume of 1.5mL, adding water until the total volume of the liquid is 1mL, and performing centrifugal purification for 3 times in a centrifuge at the rotation speed of 10000rmp to obtain a solid product, wherein the centrifugation time is 20min each time; and transferring the solid product after centrifugal purification to a vacuum drying oven to dry for 2h at the temperature of 60 ℃ to obtain the black ruthenium-iridium nano alloy.
FIG. 5 is a transmission electron microscope image showing that the Ru-Ir nano alloy prepared by the embodiment has uniform particle size distribution of about 100nm, good particle dispersibility and no agglomeration phenomenon.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing ruthenium-iridium nano alloy by utilizing laser irradiation acoustic suspension liquid drops is characterized in that ruthenium salt, iridium salt and polyvinylpyrrolidone are dissolved in ethylene glycol, then acoustic suspension treatment is carried out to obtain suspension liquid drops, and laser irradiation treatment is carried out on the suspension liquid drops to prepare the ruthenium-iridium nano alloy.
2. The method for preparing the ruthenium-iridium nano alloy by using the laser irradiation acoustic suspension liquid drop as claimed in claim 1, wherein the molar ratio of the ruthenium salt to the iridium salt is 0.05-20: 1.
3. The method for preparing the ruthenium-iridium nano alloy by using the laser irradiation acoustic suspension liquid drop as claimed in claim 1, wherein in the reaction system, the concentration of ruthenium salt is 5-100 mmol/L, and the concentration of iridium salt is 5-100 mmol/L.
4. The method for preparing the ruthenium-iridium nano alloy by using the laser irradiation acoustic suspension liquid drop as claimed in claim 1, wherein the concentration of polyvinylpyrrolidone in the reaction system is 0.1-50 g/L.
5. The method for preparing Ru-Ir nanoalloy by using laser irradiation of acoustic suspended liquid drop as claimed in claim 1, wherein the volume of the suspended liquid drop is 1-200 μ L.
6. The method for preparing the ruthenium-iridium nano alloy by using the laser irradiation acoustic suspension liquid drop as claimed in claim 1, wherein the output power of a laser is 10-80W during the laser irradiation treatment.
7. The method for preparing the ruthenium-iridium nano alloy by using the laser irradiation acoustic suspension liquid drop as claimed in claim 1, wherein the time of the laser irradiation treatment is 5-60 s.
8. The method for preparing the ruthenium-iridium nano alloy by using the laser irradiation acoustic suspension liquid drop as claimed in claim 1, wherein the suspension liquid after the laser irradiation treatment is subjected to centrifugal purification treatment.
9. The method for preparing the ruthenium-iridium nano alloy by using the laser irradiation acoustic suspension liquid drop as claimed in claim 8, wherein in the centrifugal purification treatment, the centrifugal rotation speed is 10000-13000 rpm, and the centrifugal time is 20-60 min;
or, the times of centrifugal purification treatment are 3-6 times;
or the solvent adopted in the centrifugal purification treatment is methanol, ethanol, propanol, isopropanol or water;
or drying after centrifugal purification treatment.
10. A ruthenium iridium nano alloy, which is characterized by being prepared by the method of any one of claims 1 to 9.
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| CN202011390775.6A CN112658275B (en) | 2020-12-02 | 2020-12-02 | Method for preparing ruthenium-iridium nano alloy by using laser irradiation acoustic suspension liquid drop |
| PCT/CN2021/073122 WO2022116380A1 (en) | 2020-12-02 | 2021-01-21 | Method for preparing ruthenium iridium nano alloy by means of laser irradiation and acoustic suspension of droplets |
| KR1020217040864A KR102615652B1 (en) | 2020-12-02 | 2021-01-21 | Method for manufacturing ruthenium iridium nanoalloy using laser irradiated acoustic suspension droplets |
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| CN114734051A (en) * | 2022-04-21 | 2022-07-12 | 中国科学院合肥物质科学研究院 | Method for in-situ preparation of ultra-small precious metal and non-precious metal alloy on carbon carrier |
| CN114734051B (en) * | 2022-04-21 | 2024-04-26 | 中国科学院合肥物质科学研究院 | Method for in-situ preparation of ultra-small-size noble metal non-noble metal alloy on carbon carrier |
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| CN117564289A (en) * | 2024-01-12 | 2024-02-20 | 中国科学技术大学 | Iridium ruthenium gold core-shell structure nano material and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114734051A (en) * | 2022-04-21 | 2022-07-12 | 中国科学院合肥物质科学研究院 | Method for in-situ preparation of ultra-small precious metal and non-precious metal alloy on carbon carrier |
| CN114734051B (en) * | 2022-04-21 | 2024-04-26 | 中国科学院合肥物质科学研究院 | Method for in-situ preparation of ultra-small-size noble metal non-noble metal alloy on carbon carrier |
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| KR102615652B1 (en) | 2023-12-20 |
| CN112658275B (en) | 2022-03-29 |
| KR20220079796A (en) | 2022-06-14 |
| WO2022116380A1 (en) | 2022-06-09 |
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