CN109261985A - A kind of preparation method of triangle Pt nanocrystal - Google Patents
A kind of preparation method of triangle Pt nanocrystal Download PDFInfo
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- CN109261985A CN109261985A CN201811447978.7A CN201811447978A CN109261985A CN 109261985 A CN109261985 A CN 109261985A CN 201811447978 A CN201811447978 A CN 201811447978A CN 109261985 A CN109261985 A CN 109261985A
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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
A kind of preparation method that high activity triangle is nanocrystalline, this method belongs to a kind of typical chemical method, and belong to the liquid phase preparation process in chemical method, the nanocrystalline preparation of high activity triangle can be realized on simple testing equipment by this method, products therefrom is after analysis, it was found that it is with good topography uniformity, very high catalytic activity, with important application value.Specifically, a kind of method for preparing triangle Pt nanocrystal, comprising the following steps: 1) platinum source is dispersed in the water-alcohol solution containing surfactant in water-bath；2) it is added into step 1) acquired solution and shifts to an earlier date prepared citric acid three sodium solution in right amount, magnetic agitation is uniform；3) mixed solution obtained by step 2 is transferred in hydrothermal reaction kettle, 6-12h is reacted at 120-180 DEG C, after reaction, take out reaction kettle, water cooling fast cooling；4) reaction kettle after water cooling in step 3) is opened, product can be used by centrifugation, washing.
Description
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to the preparation of noble metal nanometer material, especially one
The preparation method of kind triangle Pt nanocrystal.
Background technique
In general, so-called noble metal refers to the elements such as Au Ag Pt Pd, ruthenium, since content is less in the earth's crust for it,
Distribution do not concentrate, but catalysis, fuel cell, engineering in medicine and in terms of have important application, therefore, claimed
For noble metal.And nano material is due to effects such as its own dimensional effects, skin effect, quantum tunneling, so that its property is not
It is same as macroscopic material.Therefore, the nanosizing of noble metal is realized, this not only can be very good the advantage using nano material, may be used also
Noble metal nanometer material dosage is saved to realize, improves the effect of utilization efficiency, there is important practical usage.
In order to realize the nanosizing of precious metal material, many scientists have made a large amount of work to this, magnificent such as before 2002
(at present in the Georgia science and engineering) Xia Younan of Sheng Dun university is taught, and has been delivered on Science about silver nano-grain for the first time
Synthesis, a series of silver nano materials have been prepared by using polyol reduction method, later, and this method have been opened up
Exhibition, and successfully synthesize other kinds of noble metal nanometer material；In addition, professor Yang Peidong of University of California Berkeley is real
Show the preparation of nanowires of gold, and as template, is successfully realized the preparation of various other noble metal hybridized nanowires.Total
For, the method for synthesizing noble metal nanocrystalline now mainly includes two major classes, and one is physical methods, and one is chemical methods.It is so-called
Physical method be a kind of top-down preparation method, that is, by macroscopic view to microcosmic process, specifically include comminuting method, molecule
Beam epitaxy, evaporative condenser etc.；It is by atom to microcosmic correspondingly, so-called chemical method is a kind of preparation method from bottom to top
Process, specifically include chemical gas phase synthetic method, electrochemical process, liquid phase synthesizing method etc..Although synthetic method is varied,
With regard to the actual conditions, liquid phase synthesizing method occupy main status in all synthetic methods, this is because liquid phase synthesizing method at
This lower, easily operated, equipment for not needing complex and expensive；On the other hand, liquid phase synthesizing method passes through to reaction raw materials and reaction
The control of condition, it may be convenient to realize the separation and effectively control of nano material forming core and growth course.
When noble metal nanometer material to be used for the preparation of catalysis material, it was discovered by researchers that the table of noble metal nanometer material
Face atomic quantity and its catalytic performance have substantial connection, and general surface atom is more, and catalytic performance is stronger.If can incite somebody to action
Noble metal nanometer material is prepared into single former layer structure, and at this moment all metallic atoms are all surface atoms, and stable matches in six
Position state, has very high catalytic chemistry.Currently, the main method for preparing full active noble metals nano material is vapor deposition
Method, but there are a critical defects for this method, and since the thickness of complete active noble metal nanometer material is very thin, this makes once
Precious metal atom and substrate contact will make the separation between two-phase become abnormal difficult, in addition, the preparation of this method is expensive
Metal nano material is not easy to realize large scale preparation, and high to reaction condition requirement, therefore, at present, lacks one kind
The effectively method of preparation high activity noble metal nanometer material.
Summary of the invention
A kind of method due to lacking effectively preparation high activity noble metal nanometer material in current preparation method, the present invention
People is after a large amount of literature survey and experimental study, it is proposed that a kind of preparation method that high activity triangle is nanocrystalline, the party
It is owned by France and to belong to the liquid phase preparation process in chemical method in a kind of typical chemical method, it can simply tried by this method
It tests in equipment and realizes the nanocrystalline preparation of high activity triangle, products therefrom after analysis, finds it with good pattern
Homogeneity, very high catalytic activity have important application value.
In order to make those skilled in the art more have a clear understanding of technical solution of the present invention, now to technical solution of the present invention
Progress clearly and detailedly describes as follows.
The noble metal that we select is platinum, by taking platinum as an example, but is not limited to platinum, and those skilled in the art are of the invention in understanding
After technical solution, if only simply being changed to it, all belong to the scope of protection of the present invention within.
Specifically, a kind of method for preparing triangle Pt nanocrystal, comprising the following steps:
1) platinum source is dispersed in the water-alcohol solution containing surfactant in water-bath；
2) it is added into step 1) acquired solution and shifts to an earlier date prepared citric acid three sodium solution in right amount, magnetic agitation is uniform；
3) mixed solution obtained by step 2 is transferred in hydrothermal reaction kettle, 6-12h is reacted at 120-180 DEG C, after reaction,
Take out reaction kettle, water cooling fast cooling；
4) reaction kettle after water cooling in step 3) is opened, product can be used by centrifugation, washing.
Further, platinum source described in step 1) of the present invention includes chloroplatinic acid, platinic sodium chloride, one in acetylacetone,2,4-pentanedione platinum
Kind is several.
Further, surfactant is PVP in step 1) of the present invention, Qula is logical, one or more of CTAB.
Further, water-alcohol solution refers to deionized water, distilled water and ethyl alcohol, methanol, isopropanol in step 1) of the present invention
One of it is compound, wherein in water-alcohol solution the volume ratio of water and alcohol be 1:0.5-1.
Further, the temperature of water-bath is 30-40 DEG C in step 1) of the present invention.
Further, sodium citrate is a kind of crystal face growth regulator, concentration 0.05- in step 2 of the present invention
0.1mg/mL。
Further, platinum source in the present invention: surfactant: the mass ratio 1:5-20:0.05-0.2 of sodium citrate.
Compared with prior art, the present invention achieves following advantageous effects:
Firstly, being prepared for the method for other preparation high activity noble metal nanocrystallines at present the present invention provides a kind of
The preparation method for the noble metal nanocrystalline that method is simple, repetitive rate is high；Secondly, triangle Pt nanocrystal prepared by the present invention has
Higher catalytic activity, and the pattern prepared is more evenly；Finally, method of the invention has certain universality, Ke Yiyong
In the preparation of other noble metal nanocrystallines.
Detailed description of the invention
The TEM photo of triangle Pt nanocrystal prepared by Fig. 1 embodiment of the present invention 1；
The TEM photo of triangle Pt nanocrystal prepared by Fig. 2 embodiment of the present invention 2；
The TEM photo of triangle Pt nanocrystal prepared by Fig. 3 embodiment of the present invention 3；
The TEM photo of Pt nanocrystal prepared by Fig. 4 comparative example 1 of the present invention；
It is to be appreciated that in figs 1-3, the irregular substance occurred in visual field belongs to the impurity not cleaned up.
Specific embodiment
Technical solution in the embodiment of the present invention is purged complete description below, it is clear that described implementation
Example is only a part of the embodiments of the present invention, and based on the embodiments of the present invention, those skilled in the art are original
On the basis of improvement, belong to protection scope of the present invention.
A method of preparing triangle Pt nanocrystal, comprising the following steps:
1) platinum source is dispersed in the water-alcohol solution containing surfactant in water-bath；
2) it is added into step 1) acquired solution and shifts to an earlier date prepared citric acid three sodium solution in right amount, magnetic agitation is uniform；
3) mixed solution obtained by step 2 is transferred in hydrothermal reaction kettle, 6-12h is reacted at 120-180 DEG C, after reaction,
Take out reaction kettle, water cooling fast cooling；
4) reaction kettle after water cooling in step 3) is opened, product can be used by centrifugation, washing.
Further, platinum source described in step 1) of the present invention includes chloroplatinic acid, platinic sodium chloride, one in acetylacetone,2,4-pentanedione platinum
Kind is several.
Further, surfactant is PVP in step 1) of the present invention, Qula is logical, one or more of CTAB.
Further, water-alcohol solution refers to deionized water, distilled water and ethyl alcohol, methanol, isopropanol in step 1) of the present invention
One of it is compound, wherein in the ratio of water-alcohol solution the volume ratio of water and alcohol be 1:0.5-1.
Further, the temperature of water-bath is 30-40 DEG C in step 1) of the present invention.
Further, sodium citrate is a kind of crystal face growth regulator, concentration 0.05- in step 2 of the present invention
0.1mg/mL。
Further, platinum source in the present invention: surfactant: the mass ratio 1:5-20:0.05-0.2 of sodium citrate.It is more excellent
It is selected as 1:5-10:0.05-0.1.
Embodiment 1
Water-bath is warming up to 30 DEG C, 1g chloroplatinic acid is added into the PVP water-alcohol solution that concentration is 20mg/mL, wherein water alcohol is molten
Liquid is the mixed solution of deionized water and ethyl alcohol, volume ratio 1:0.5；Keep the temperature 10min after, then by 1mL concentration be 0.05mg/
The sodium citrate of mL, which is added thereto, to stir evenly；Later, which is transferred in hydrothermal reaction kettle, it is anti-at 160 DEG C
10h is answered, after reaction, through hydro-thermal, centrifugation and carrying out washing treatment.
Embodiment 2
Water-bath is warming up to 30 DEG C, 1g chloroplatinic acid is added into the PVP water-alcohol solution that concentration is 20mg/mL, wherein water alcohol is molten
Liquid is the mixed solution of deionized water and methanol, volume ratio 1:1；Keep the temperature 10min after, then by 1mL concentration be 0.05mg/mL
Sodium citrate be added thereto and stir evenly；Later, which is transferred in hydrothermal reaction kettle, is reacted at 160 DEG C
10h, after reaction, through hydro-thermal, centrifugation and carrying out washing treatment.
Embodiment 3
Water-bath is warming up to 30 DEG C, 1g acetylacetone,2,4-pentanedione platinum is added into the PVP water-alcohol solution that concentration is 20mg/mL, wherein water
Alcoholic solution is the mixed solution of deionized water and isopropanol, volume ratio 1:0.5；After keeping the temperature 10min, then by 2mL concentration it is
The sodium citrate of 0.05mg/mL, which is added thereto, to stir evenly；Later, which is transferred in hydrothermal reaction kettle, 180
6h is reacted at DEG C, after reaction, through hydro-thermal, centrifugation and carrying out washing treatment.
Embodiment 4
Water-bath is warming up to 30 DEG C, 1g chloroplatinic acid is added into PVP the and CTAB mixing water-alcohol solution that concentration is 20mg/mL,
Wherein, water-alcohol solution is the mixed solution of deionized water and ethyl alcohol, volume ratio 1:1；After keeping the temperature 10min, then by 2mL concentration
It is added thereto and stirs evenly for the sodium citrate of 0.05mg/mL；Later, which is transferred in hydrothermal reaction kettle,
10h is reacted at 160 DEG C, after reaction, through hydro-thermal, centrifugation and carrying out washing treatment.
Embodiment 5
Water-bath is warming up to 40 DEG C, 1g chloroplatinic acid is added into PVP the and CTAB mixing water-alcohol solution that concentration is 20mg/mL,
Wherein, water-alcohol solution is the mixed solution of deionized water and isopropanol, volume ratio 1:0.5；After keeping the temperature 10min, then by 1mL
Concentration is added thereto for the sodium citrate of 0.05mg/mL and stirs evenly；Later, which is transferred to hydrothermal reaction kettle
In, 6h is reacted at 160 DEG C, after reaction, through hydro-thermal, centrifugation and carrying out washing treatment.
Comparative example 1
Other conditions are only not added with sodium citrate solution with embodiment 1, difference in reaction solution.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from invention
Design or beyond the scope defined by this claim, be within the scope of protection of the invention.
Claims (7)
1. a kind of preparation method of triangle Pt nanocrystal, it is characterised in that: the following steps are included: 1) by platinum source in water-bath
It is dispersed in the water-alcohol solution containing surfactant；
2) it is added into step 1) acquired solution and shifts to an earlier date prepared citric acid three sodium solution in right amount, magnetic agitation is uniform；
3) mixed solution obtained by step 2 is transferred in hydrothermal reaction kettle, 6-12h is reacted at 120-180 DEG C, after reaction,
Take out reaction kettle, water cooling fast cooling；
4) reaction kettle after water cooling in step 3) is opened, product can be used by centrifugation, washing.
2. a kind of preparation method of triangle Pt nanocrystal according to claim 1, it is characterised in that: described in step 1)
Platinum source include one or more of chloroplatinic acid, platinic sodium chloride, acetylacetone,2,4-pentanedione platinum.
3. a kind of preparation method of triangle Pt nanocrystal according to claim 1, it is characterised in that: surface in step 1)
Activating agent is PVP, Qula is logical, one or more of CTAB.
4. a kind of preparation method of triangle Pt nanocrystal according to claim 1, it is characterised in that: water alcohol in step 1)
Solution refers to the compound of one of deionized water, distilled water and ethyl alcohol, methanol, isopropanol, wherein in the ratio of water-alcohol solution
The volume ratio of water and alcohol is 1:0.5-1.
5. a kind of preparation method of triangle Pt nanocrystal according to claim 1, it is characterised in that: lemon in step 2
Sour sodium is a kind of crystal face growth regulator, concentration 0.05-0.1mg/mL.
6. a kind of preparation method of triangle Pt nanocrystal according to claim 1, it is characterised in that: the platinum source:
Surfactant: the mass ratio 1:5-20:0.05-0.2 of sodium citrate.More preferably 1:5-10:0.05-0.1.
7. triangle Pt nanocrystal prepared by claim 1-6 any claim is used for fuel battery negative pole oxygen catalytic
Reduction reaction.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111069625A (en) * | 2020-01-06 | 2020-04-28 | 昆明理工大学 | Preparation method of flaky platinum nanoparticles |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111069625A (en) * | 2020-01-06 | 2020-04-28 | 昆明理工大学 | Preparation method of flaky platinum nanoparticles |
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