CN105798325B - A kind of ruthenium (Ru) nanometer line network of Asia 2nm and preparation method thereof - Google Patents
A kind of ruthenium (Ru) nanometer line network of Asia 2nm and preparation method thereof Download PDFInfo
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- CN105798325B CN105798325B CN201610170409.7A CN201610170409A CN105798325B CN 105798325 B CN105798325 B CN 105798325B CN 201610170409 A CN201610170409 A CN 201610170409A CN 105798325 B CN105798325 B CN 105798325B
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- ruthenium
- asia
- nanometer line
- line network
- reducing agent
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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 kind of ruthenium (Ru) nanometer line networks and its synthetic method of Asia 2nm, it is characterised in that：(1) surfactant and reducing agent are added to the water together, stirred 3~5 minutes at room temperature, the mass ratio of surfactant and reducing agent is 1:2~2:1；Institute's amount of water needs surfactant and reducing agent being completely dissolved；(2) ratio of the addition metal Ru salt precursor liquid solution into mixed solution obtained by step (1), added water and ruthenium precursor solution is 5:1~10:1；A concentration of 0.05~0.5mol/L of ruthenium metal precursor；It stirs 1~3 minute at room temperature；(3) mixed solution obtained by step (2) is transferred in autoclave and reacted 12~30 hours, temperature is controlled at 150~200 DEG C；(4) it is washed after step (3) products therefrom is cooled down, up to a kind of Ru nanometer line networks of Asia 2nm after centrifugation.
Description
Technical field
The present invention relates to ruthenium (Ru) nanometer line networks and its synthetic method that a kind of diameter is less than 2nm.
Background technology
As the important element in Pt races metal, Ru is in oxidation of alcohols, nitrogen fixation, biomass fuel and liquid fuel electricity
It does not replace in pond etc..The inner link of structure and performance determines the size of metal nanocrystal and pattern control
It makes particularly significant.Compared with other Pt races metal, such as Pd, Pt, Rh, the pattern control technologies of Ru nanocrystals also less into
It is ripe, the reported synthetic method that spherical Ru nano particles are only synthesized in organic media.
In recent years, one-dimensional nano line caused the extensive concern of scientific circles due to its unique structure and performance.And solution
The nanowire diameter of system synthesis is often relatively large (＞ 5nm), and the nano wire ability of several years Asia 2nm is in oleyl amine phase up to date
It is synthesized.Therefore synthesis only has several atom thicknesses even to have important meaning close to ruthenium (Ru) nano wire of a lattice unit
Justice.
Invention content
The technical problem to be solved by the present invention is to：A kind of ruthenium (Ru) nanometer line network of diameter less than 2nm and its conjunction are provided
Into method.
The technical scheme is that：A kind of preparation method of ruthenium (Ru) nanometer line network of Asia 2nm, includes following step
Suddenly：
(1) surfactant and reducing agent are added to the water together, stirred 3~5 minutes at room temperature, surfactant is with going back
The mass ratio of former agent is 1:2~2:1；Institute's amount of water needs surfactant and reducing agent being completely dissolved；
(2) metal Ru salt precursor liquid solution, added water and ruthenium precursor solution are added in into mixed solution obtained by step (1)
Ratio be 5:1~10:1；A concentration of 0.05~0.5mol/L of ruthenium metal precursor；It stirs 1~3 minute at room temperature；
(3) mixed solution obtained by step (2) is transferred in autoclave and reacted 12~30 hours, temperature control exists
150~200 DEG C；
(4) it washs after step (3) products therefrom is cooled down, is received after centrifugation up to a kind of ruthenium (Ru) of Asia 2nm
Nanowire network.
Aqueous solution described in step (1) is ultra-pure water, and mixing time is 5 minutes, surfactant and reducing agent quality
Than being 1:1.
Surfactant is the mixture of SDS and KF in step (1)；Reducing agent is PVP (MW=40 000).
Metal Ru salt precursor liquid solution described in step (2) is ruthenium trichloride.
It is stirred at room temperature described in step (2) 1 minute.
At 180 DEG C, the reaction time is 20 hours for reaction temperature control in autoclave described in step (3).
Beneficial effects of the present invention：It is average straight present invention obtains a kind of unitary ruthenium (Ru) nanometer line network of Asia 2nm
Diameter controls product morphology, pattern is unified, structure novel, while yield is higher in 1.5 ± 0.2nm well.
Description of the drawings
Fig. 1 is ruthenium (Ru) nanometer line network transmission electron microscope observation result figure of Asia 2nm；
Ruthenium (Ru) the nanometer line network high resolution transmission electron microscope that Fig. 2 is Asia 2nm observes result figure；
Fig. 3 is the X-ray diffractogram of ruthenium (Ru) nanometer line network of Asia 2nm.
Specific embodiment
Embodiment 1
(1) it is 1 in mass ratio by surfactant and reducing agent:1 adds in aqueous solution, stirs 5 minutes；
(2) solution of ruthenium trichloride of a concentration of 0.1mol/L, room temperature are added in into mixed solution (7ml) obtained by step (1)
Stirring 1 minute；Mixed solution colour is peony；
(3) mixed solution obtained by step (2) is transferred in autoclave and reacted 15 hours, temperature is controlled at 180 DEG C；
(4) by step (3) products therefrom cooling, centrifuge and with deionized water carries out three times wash after distributed and saved in
In ethanol solution.Product is worm shape nano wire and a small number of short grained mixtures, and nano wire starts branch occur.
Embodiment 2
(1) it is 1 in mass ratio by surfactant and reducing agent:2 add in aqueous solution, stir 3 minutes；
(2) solution of ruthenium trichloride of a concentration of 0.1mol/L, room temperature are added in into mixed solution (7ml) obtained by step (1)
Stirring 2 minutes；Mixed solution colour is peony；
(3) mixed solution obtained by step (2) is transferred in autoclave and reacted 18 hours, temperature is controlled at 180 DEG C；
(4) by step (3) products therefrom cooling, centrifuge and with deionized water carries out three times wash after distributed and saved in
In ethanol solution.Product is longer and more branch nano wire and part nanometer line network.
Embodiment 3
(1) it is 2 in mass ratio by surfactant and reducing agent:1 adds in aqueous solution, stirs 4 minutes；
(2) solution of ruthenium trichloride of a concentration of 0.1mol/L, room temperature are added in into mixed solution (7ml) obtained by step (1)
Stirring 3 minutes；Mixed solution colour is peony；
(3) mixed solution obtained by step (2) is transferred in autoclave and reacted 24 hours, temperature is controlled at 180 DEG C；
(4) by step (3) products therefrom cooling, centrifuge and with deionized water carries out three times wash after distributed and saved in
In ethanol solution.The nanometer line network that product is formed for the more nano wires of longer and branch.
Fig. 1 are ruthenium (Ru) nano wire transmission electron microscope observation result figures of sub- 2nm.It can be seen that product is mutual
The network that the superfine nano wire being connected is formed.
Fig. 2 are ruthenium (Ru) the nano wire high resolution transmission electron microscope observation result figures of sub- 2nm.It can be seen that
The average diameter of product nano line is in 1.5 ± 0.2nm.
Fig. 3 are the X-ray diffractograms of ruthenium (Ru) nano wire of sub- 2nm, it can be seen that only there are one positioned at 42.4 ° plus
Wide characteristic peak is consistent with product for minor diameter Ru nanometer line networks.
Claims (5)
1. a kind of ruthenium of Asia 2nm（Ru）The preparation method of nanometer line network, it is characterised in that：It comprises the steps of：（1）By table
Face activating agent and reducing agent are added to the water together, stir 3~5 minutes at room temperature, the mass ratio of surfactant and reducing agent
It is 1:2~2:1；Institute's amount of water needs surfactant and reducing agent being completely dissolved；（2）To step（1）Gained mixes
The ratio of addition metal Ru salt precursor liquid solution in solution, added water and metal Ru salt precursor liquid solution is 5:1~10:1；Gold
Belong to a concentration of 0.05~0.5mol/L of ruthenium salt precursor body；It stirs 1~3 minute at room temperature；（3）By step（2）Gained mixes
Solution, which is transferred in autoclave, to react 12~30 hours, and temperature is controlled at 150~200 DEG C；（4）By step（3）Gained
It is washed after product cooling, up to a kind of ruthenium of Asia 2nm after centrifugation（Ru）Nanometer line network；Surface is lived in step (1)
Property agent be SDS and KF mixture；Reducing agent is PVP.
2. a kind of ruthenium of Asia 2nm according to claim 1（Ru）The preparation method of nanometer line network, feature exist
In：Water described in step (1) is ultra-pure water, and mixing time is 5 minutes, and surfactant is 1 with reducing agent mass ratio:
1。
3. a kind of ruthenium of Asia 2nm according to claim 1（Ru）The preparation method of nanometer line network, feature exist
In：Metal Ru salt precursor liquid solution described in step (2) is ruthenium trichloride.
4. a kind of ruthenium of Asia 2nm according to claim 1（Ru）The preparation method of nanometer line network, feature exist
In：It is stirred at room temperature described in step (2) 1 minute.
5. a kind of ruthenium of Asia 2nm according to claim 1（Ru）The preparation method of nanometer line network, feature exist
In：At 180 DEG C, the reaction time is 20 hours for reaction temperature control in autoclave in step (3).
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| CN105798325B true CN105798325B (en) | 2018-07-06 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN110625136B (en) * | 2019-10-14 | 2022-04-22 | 商丘师范学院 | Method for efficiently and simply synthesizing Ru nanowire |
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104998636A (en) * | 2015-07-29 | 2015-10-28 | 贵州大学 | Synthetic method and application of PtRu binary metal nano-alloy catalyst |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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