CN105798325A - Sub-2nm ruthenium (Ru) nanowire network and preparation method thereof - Google Patents
Sub-2nm ruthenium (Ru) nanowire network and preparation method thereof Download PDFInfo
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- CN105798325A CN105798325A CN201610170409.7A CN201610170409A CN105798325A CN 105798325 A CN105798325 A CN 105798325A CN 201610170409 A CN201610170409 A CN 201610170409A CN 105798325 A CN105798325 A CN 105798325A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a sub-2nm ruthenium (Ru) nanowire network and a synthesis method thereof. The method is characterized by comprising the following steps: (1) a surface active agent and a reducing agent are added in water for stirring for 3-5 minutes at room temperature; the mass ratio of the surface active agent to the reducing agent is 1: 2-2: 1; and the quantity of the added water needs to meet the condition that the added water can totally dissolve the surface active agent and the reducing agent; (2) metal ruthenium salt precursor solution is added in the obtained mixed solution in the step (1) for stirring for 1-3 minutes at room temperature; the ratio of the added water to the ruthenium precursor solution is 5: 1-10: 1; and the concentration of the ruthenium metal precursor is 0.05-0.5 mol/L; (3) the mixed solution obtained in the step (2) is transferred into a high-pressure reaction kettle for reacting for 12-30 hours; and the temperature is controlled within 150-200 DEG C; and (4) the product obtained in the step (3) is cooled for washing, and is centrifugally separated to obtain the sub-2nm Ru nanowire network.
Description
The present invention relates to a kind of diameter ruthenium (Ru) nanometer line network less than 2nm and synthetic method thereof.
Background technology
As the important element in Pt race metal, Ru has, in oxidation of alcohols, nitrogen fixation, biomass fuel and liquid fuel battery etc., the effect do not replaced.The internal relation of structure and performance determines that the size of metal nanocrystal and morphology control are particularly significant.With other Pt race metal, as Pd, Pt, Rh etc. compare, the morphology control technology of Ru nanocrystal is also not overripened, the reported synthetic method only synthesizing spherical Ru nano-particle in organic media.
In recent years, one-dimensional nano line caused the extensive concern of scientific circles due to the structure of its uniqueness and performance.And the nanowire diameter of solution system synthesis is often relatively large (> 5nm), the nano wire of several years up to date sub-2nm just oleyl amine mutually in be synthesized.Therefore only several atom thicknesses are even significant close to ruthenium (Ru) nano wire of a lattice unit in synthesis.
Summary of the invention
The technical problem to be solved in the present invention is: provide a kind of diameter ruthenium (Ru) nanometer line network less than 2nm and synthetic method thereof.
The preparation method that the technical scheme is that ruthenium (Ru) nanometer line network of a kind of sub-2nm, comprises the steps of
(1) being added to the water together with reducing agent by surfactant, stir 3～5 minutes under room temperature, the mass ratio of surfactant and reducing agent is 1:2～2:1；Institute's amount of water needs to be completely dissolved surfactant and reducing agent；
(2) adding metal Ru salt precursor liquid solution in step (1) gained mixed solution, the ratio with ruthenium precursor solution that added water is 5:1～10:1；The concentration of ruthenium metal precursor is 0.05～0.5mol/L；Stir 1～3 minute under room temperature；
(3) being transferred to by step (2) gained mixed solution in autoclave and react 12～30 hours, temperature controls at 150～200 DEG C；
(4) wash after step (3) products therefrom being cooled down, after centrifugation, namely obtain ruthenium (Ru) nanometer line network of a kind of sub-2nm.
Aqueous solution described in step (1) is ultra-pure water, and mixing time is 5 minutes, and surfactant and reducing agent mass ratio are 1:1.
In step (1), surfactant is the mixture of SDS and KF；Reducing agent is PVP (MW=40000).
Metal Ru salt precursor liquid solution described in step (2) is ruthenium trichloride.
Stir 1 minute under room temperature described in step (2).
Described in step (3), in autoclave, reaction temperature controls at 180 DEG C, and the response time is 20 hours.
Beneficial effects of the present invention: present invention obtains unitary ruthenium (Ru) nanometer line network of a kind of sub-2nm, average diameter, at 1.5 ± 0.2nm, well controls product morphology, and pattern is unified, novel structure, and yield is higher simultaneously.
Accompanying drawing explanation
Fig. 1 is ruthenium (Ru) the nanometer line network transmission electron microscope observation result figure of sub-2nm；
Fig. 2 is ruthenium (Ru) the nanometer line network high resolution transmission electron microscope observed result figure of sub-2nm；
Fig. 3 is the X-ray diffractogram of ruthenium (Ru) nanometer line network of sub-2nm.
Detailed description of the invention
Embodiment 1
(1) surfactant is added in aqueous solution for 1:1 in mass ratio with reducing agent, stir 5 minutes；
(2) adding concentration in step (1) gained mixed solution (7ml) is the solution of ruthenium trichloride of 0.1mol/L, is stirred at room temperature 1 minute；Mixed solution colour is peony；
(3) being transferred to by step (2) gained mixed solution in autoclave and react 15 hours, temperature controls at 180 DEG C；
(4) by step (3) products therefrom cool down, centrifugation and with deionized water carry out three times washing after distributed and saved in alcoholic solution.Product is worm shape nano wire and the short grained mixture of minority, and nano wire starts branch occur.
Embodiment 2
(1) surfactant is added in aqueous solution for 1:2 in mass ratio with reducing agent, stir 3 minutes；
(2) adding concentration in step (1) gained mixed solution (7ml) is the solution of ruthenium trichloride of 0.1mol/L, is stirred at room temperature 2 minutes；Mixed solution colour is peony；
(3) being transferred to by step (2) gained mixed solution in autoclave and react 18 hours, temperature controls at 180 DEG C；
(4) by step (3) products therefrom cool down, centrifugation and with deionized water carry out three times washing after distributed and saved in alcoholic solution.Product is longer and that branch is more nano wire and part nanometer line network.
Embodiment 3
(1) surfactant is added in aqueous solution for 2:1 in mass ratio with reducing agent, stir 4 minutes；
(2) adding concentration in step (1) gained mixed solution (7ml) is the solution of ruthenium trichloride of 0.1mol/L, is stirred at room temperature 3 minutes；Mixed solution colour is peony；
(3) being transferred to by step (2) gained mixed solution in autoclave and react 24 hours, temperature controls at 180 DEG C；
(4) by step (3) products therefrom cool down, centrifugation and with deionized water carry out three times washing after distributed and saved in alcoholic solution.Product is longer and the nanometer line network of the more nano wire composition of branch.
Fig. 1. it is ruthenium (Ru) the nano wire transmission electron microscope observation result figure of sub-2nm.Can be seen that product is the network that the superfine nano wire interconnected is constituted.
Fig. 2. it is ruthenium (Ru) the nano wire high resolution transmission electron microscope observed result figure of sub-2nm.Can be seen that the average diameter of product nano line is at 1.5 ± 0.2nm.
Fig. 3. it is the X-ray diffractogram of ruthenium (Ru) nano wire of sub-2nm, it can be seen that only one of which is positioned at the characteristic peak widened of 42.4 °, is that minor diameter Ru nanometer line network is consistent with product.
Claims (6)
1. the preparation method of ruthenium (Ru) nanometer line network of a sub-2nm, it is characterised in that: comprise the steps of
(1) being added to the water together with reducing agent by surfactant, stir 3～5 minutes under room temperature, the mass ratio of surfactant and reducing agent is 1:2～2:1；Institute's amount of water needs to be completely dissolved surfactant and reducing agent；
(2) adding metal Ru salt precursor liquid solution in step (1) gained mixed solution, the ratio with ruthenium precursor solution that added water is 5:1～10:1；The concentration of ruthenium metal precursor is 0.05～0.5mol/L；Stir 1～3 minute under room temperature；
(3) being transferred to by step (2) gained mixed solution in autoclave and react 12～30 hours, temperature controls at 150～200 DEG C；
(4) wash after step (3) products therefrom being cooled down, after centrifugation, namely obtain ruthenium (Ru) nanometer line network of a kind of sub-2nm.
2. the preparation method of ruthenium (Ru) nanometer line network of a kind of sub-2nm according to claim 1, it is characterized in that: the aqueous solution described in step (1) is ultra-pure water, mixing time is 5 minutes, and surfactant and reducing agent mass ratio are 1:1.
3. the preparation method of ruthenium (Ru) nanometer line network of a kind of sub-2nm according to claim 1, it is characterised in that: in step (1), surfactant is the mixture of SDS and KF；Reducing agent is PVP.
4. the preparation method of ruthenium (Ru) nanometer line network of a kind of sub-2nm according to claim 1, it is characterised in that: the metal Ru salt precursor liquid solution described in step (2) is ruthenium trichloride.
5. the preparation method of ruthenium (Ru) nanometer line network of a kind of sub-2nm according to claim 1, it is characterised in that: stir 1 minute under room temperature described in step (2).
6. the preparation method of ruthenium (Ru) nanometer line network of a kind of sub-2nm according to claim 1, it is characterised in that: described in step (3), in autoclave, reaction temperature controls at 180 DEG C, and the response time is 20 hours.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110625135A (en) * | 2019-10-14 | 2019-12-31 | 商丘师范学院 | Method for efficiently, simply and easily synthesizing Ru nanocrystals with different morphologies |
| CN110625136A (en) * | 2019-10-14 | 2019-12-31 | 商丘师范学院 | Method for efficiently and simply synthesizing Ru nanowire |
| CN111359607A (en) * | 2020-03-09 | 2020-07-03 | 安徽师范大学 | Titanium dioxide loaded nanoscale Ru metal short wire composite material and preparation method and application thereof |
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| CN1237494A (en) * | 1998-05-29 | 1999-12-08 | 中国科学院化学研究所 | Preparation of metal nanometre cluster |
| CN1903427A (en) * | 2005-07-28 | 2007-01-31 | 中国科学院大连化学物理研究所 | Method for preparing metal ruthenium nano-wire |
| CN101530922A (en) * | 2009-04-13 | 2009-09-16 | 西安交通大学 | Method for preparing one-dimensional alloy nanometer wire |
| CN102560415A (en) * | 2012-01-20 | 2012-07-11 | 中国科学院上海硅酸盐研究所 | Three-dimensional graphene/metal line or metal wire composite structure and preparation method thereof |
| US20130084210A1 (en) * | 2011-09-30 | 2013-04-04 | The Research Foundation Of State University Of New York | Surfactantless metallic nanostructures and method for synthesizing same |
| CN104998636A (en) * | 2015-07-29 | 2015-10-28 | 贵州大学 | Synthetic method and application of PtRu binary metal nano-alloy catalyst |
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2016
- 2016-03-24 CN CN201610170409.7A patent/CN105798325B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1237494A (en) * | 1998-05-29 | 1999-12-08 | 中国科学院化学研究所 | Preparation of metal nanometre cluster |
| CN1903427A (en) * | 2005-07-28 | 2007-01-31 | 中国科学院大连化学物理研究所 | Method for preparing metal ruthenium nano-wire |
| CN101530922A (en) * | 2009-04-13 | 2009-09-16 | 西安交通大学 | Method for preparing one-dimensional alloy nanometer wire |
| US20130084210A1 (en) * | 2011-09-30 | 2013-04-04 | The Research Foundation Of State University Of New York | Surfactantless metallic nanostructures and method for synthesizing same |
| CN102560415A (en) * | 2012-01-20 | 2012-07-11 | 中国科学院上海硅酸盐研究所 | Three-dimensional graphene/metal line or metal wire composite structure and preparation method thereof |
| CN104998636A (en) * | 2015-07-29 | 2015-10-28 | 贵州大学 | Synthetic method and application of PtRu binary metal nano-alloy catalyst |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110625135A (en) * | 2019-10-14 | 2019-12-31 | 商丘师范学院 | Method for efficiently, simply and easily synthesizing Ru nanocrystals with different morphologies |
| CN110625136A (en) * | 2019-10-14 | 2019-12-31 | 商丘师范学院 | Method for efficiently and simply synthesizing Ru nanowire |
| CN110625136B (en) * | 2019-10-14 | 2022-04-22 | 商丘师范学院 | Method for efficiently and simply synthesizing Ru nanowire |
| CN110625135B (en) * | 2019-10-14 | 2022-04-22 | 商丘师范学院 | Method for efficiently, simply and easily synthesizing Ru nanocrystals with different morphologies |
| CN111359607A (en) * | 2020-03-09 | 2020-07-03 | 安徽师范大学 | Titanium dioxide loaded nanoscale Ru metal short wire composite material and preparation method and application thereof |
| CN111359607B (en) * | 2020-03-09 | 2022-03-15 | 安徽师范大学 | Titanium dioxide loaded nanoscale Ru metal short wire composite material and preparation method and application thereof |
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