CN106180751B - A kind of nanometer platinum-nickel alloy and its preparation and application - Google Patents
A kind of nanometer platinum-nickel alloy and its preparation and application Download PDFInfo
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- CN106180751B CN106180751B CN201610629815.5A CN201610629815A CN106180751B CN 106180751 B CN106180751 B CN 106180751B CN 201610629815 A CN201610629815 A CN 201610629815A CN 106180751 B CN106180751 B CN 106180751B
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Abstract
The invention discloses a kind of nanometer platinum-nickel alloy and its preparation and application, it is related to nanocatalyst technical field, the present invention first mixes chloroplatinic acid and nickel chloride in proportion, add PVP, then after adjusting pH value of solution, add reducing agent, pass through strict controlling reaction temperature and reaction time, obtain the alloy catalyst of morphology and history and size uniform, the present invention passes through the synergy between metal platinum and metallic nickel, improve the activity and electrocatalysis characteristic of metal, reduce the usage amount of noble metal platinum, reduce cost, and the preparation method of platinum-nickel alloy is simple, it is gentle controllable, too high temperature and harsh experiment condition are not needed, stable experiment is good, yield is high.
Description
Technical field
The present invention relates to nanocatalyst technical field, and in particular to a kind of nanometer platinum-nickel alloy and its preparation and application.
Background technology
With the fast development of society, energy demand makes the mankind be badly in need of the subject matter solved, and fuel cell makes a kind of clear
The clean energy, it is recognized as making the most promising energy, in the catalytic oxidation of methanol, metal platinum is low because being coordinated between its atom
It is relatively low with the avtive spot that rides over nanoparticle surface, be advantageous to the electroxidation of organic molecule and the decomposition of water, show compared with
High catalytic activity, an alloy particle with the controllable micro nano structure of multi phase interface structure and surface is started, however,
Platinum is not only expensive but also stability is poor, hinders its extensive use on fuel cell.Therefore, it is a kind of novel to find
Alternative metal platinum is just particularly important to improve the material of its catalytic performance.
Alloy material can print and distribute series of effects, such as the isolation of surface-element, the change of geometric configuration and platinum electricity
The change of minor structure, so as to improve the electro catalytic activity of platinum.In these alloy catalysts, platinum base transition metal nano material
Extensive concern is caused, this is mainly due to their excellent optics, electricity, magnetics and catalytic performances, is bonded with platinum
Bimetallic catalyst there is bimetallic synergy, so as to substantially increase the electrocatalysis characteristic of metal platinum, result of study table
Bright, platinum bimetallic alloy film made from electro-deposition is compared with the pure platinum catalyst that electro-deposition obtains, bimetallic alloy catalyst
Significantly improve the redox efficiency of methanol.But in the prior art, the method for preparing platinum-nickel alloy is extremely harsh, prepares bar
Part is difficult to control, and prepares low yield, and poor repeatability, the component of resulting alloy particle is uneven, and particle size is difficult to control,
The alloy catalyst tool that dimension finds a kind of component size uniform is of great significance.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of platinum-nickel alloy particle of component size uniform, it has
Excellent catalytic effect, stable performance, the characteristics of preparation method is simple.
To realize object above, the present invention is achieved by the following technical programs：
The preparation method of a kind of nanometer of platinum-nickel alloy, comprises the following steps：
(1) surfactant is dissolved in organic solution, obtains solution A；
(2) 1g chloroplatinic acids are dissolved in 100mL water, then add 2~5mL0.1mol/L nickel chloride aqueous solutions thereto,
Then 5~8g PVP are added into mixed system again, stirs to being completely dissolved, obtains solution B；
(3) solution A is added in solution B, adds sodium chloride, after stirring, added alkaline solution, adjust pH to 9
~12, then it is placed in ice-water bath；
(4) 0.5mol/L NaHB solution is added dropwise into the mixed system of step (3), and system is slowly stirred, drips
After adding end, mixed solution is warming up to 50~70 DEG C, and is incubated 24~72h, obtains granular disintegration；
(5) after granular disintegration is cleaned with saturated sodium-chloride, then cleaned with ethanol, Platinum Nanoparticles nickel is obtained after vacuum drying
Alloy.
Preferably, the organic solvent is one kind in ethanol, ethylene glycol, isopropanol.
Preferably, the surfactant is cetyl trimethylammonium bromide, tetrabutyl phosphonium bromide phosphine, TBAB
In one kind.
Preferably, the concentration of the surfactant solution is 0.01~0.05mol/L.
Preferably, the mean molecule quantity of the PVP is 40000.
Preferably, the alkaline solution is sodium hydroxide solution, sodium carbonate liquor, one kind in sodium bicarbonate solution or more
Kind composition.
A kind of nanometer platinum-nickel alloy, the wherein mol ratio of platinum and nickel are 4~10:1, its grain diameter is 10~20nm.
The present invention also provides the application of a kind of nanometer of platinum-nickel alloy, and the nanometer platinum-nickel alloy can be used for methanol fuel cell
Catalyst.
Beneficial effects of the present invention：Platinum-nickel alloy provided by the invention, due to the synergy between metal platinum and metallic nickel,
The activity and electrocatalysis characteristic of metal are improved, reduces the usage amount of noble metal platinum, improves the utilization rate of catalyst, is reduced
Cost, and alloy has homogeneous size and institutional framework, also with larger specific surface area, to the catalysis oxidation of methanol
With significant effect, and the preparation method of platinum-nickel alloy is simple, gentle controllable, it is not necessary to too high temperature and harsh experiment
Condition, stable experiment is good, yield is high.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making
The every other embodiment obtained under the premise of creative work, belongs to the scope of protection of the invention.
Embodiment 1：
A kind of preparation method of Platinum Nanoparticles nickel alloy catalyst for direct methanol dye cell, comprises the following steps：
(1) 1mmol cetyl trimethylammonium bromides are dissolved in 20mL ethylene glycol, obtain solution A；
(2) 1g chloroplatinic acids are dissolved in 100mL water, the chloroplatinic acid aqueous solution that concentration is 0.0193mol/L are obtained, then to it
Middle addition 2.5mL 0.1mol/L nickel chloride aqueous solutions, 6g PVP (Mw=40000), stirring are then added into mixed system again
To being completely dissolved, solution B is obtained；
(3) solution A is added in solution B, adds sodium chloride, after stirring, add sodium carbonate and sodium hydroxide
Mixed solution, pH to 10 is adjusted, is then placed in ice-water bath；
(4) 0.5mol/L NaHB solution is added dropwise into the mixed system of step (3), and system is slowly stirred, drips
After adding end, mixed solution is warming up to 60 DEG C, and is incubated 60h, obtains granular disintegration；
(5) after granular disintegration is cleaned with saturated sodium-chloride, then cleaned with ethanol, particle diameter is obtained after vacuum drying is
The mol ratio of 10nm platinum-nickel alloy, wherein platinum and nickel is 5:1.
Embodiment 2：
A kind of preparation method of Platinum Nanoparticles nickel alloy catalyst for direct methanol dye cell, comprises the following steps：
(1) 0.05mmol cetyl trimethylammonium bromides are dissolved in 20mL ethanol, obtain solution A；
(2) 1g chloroplatinic acids are dissolved in 100mL water, the chloroplatinic acid aqueous solution that concentration is 0.0193mol/L are obtained, then to it
Middle addition 2mL 0.1mol/L nickel chloride aqueous solutions, 5g PVP (Mw=40000) are then added into mixed system again, stirring is extremely
It is completely dissolved, obtains solution B；
(3) solution A is added in solution B, adds sodium chloride, after stirring, added sodium hydroxide solution, adjust pH
To 12, then it is placed in ice-water bath；
(4) 0.5mol/L NaHB solution is added dropwise into the mixed system of step (3), and system is slowly stirred, drips
After adding end, mixed solution is warming up to 70 DEG C, and is incubated 24h, obtains granular disintegration；
(5) after granular disintegration is cleaned with saturated sodium-chloride, then cleaned with ethanol, particle diameter is obtained after vacuum drying is
The mol ratio of 15nm platinum-nickel alloy, wherein platinum and nickel is 10:1.
Embodiment 3：
A kind of preparation method of Platinum Nanoparticles nickel alloy catalyst for direct methanol dye cell, comprises the following steps：
(1) 0.04mmol tetrabutyl phosphonium bromide phosphines are dissolved in 20mL ethylene glycol, obtain solution A；
(2) 1g chloroplatinic acids are dissolved in 100mL water, the chloroplatinic acid aqueous solution that concentration is 0.0193mol/L are obtained, then to it
Middle addition 5mL 0.1mol/L nickel chloride aqueous solutions, 6g PVP (Mw=40000) are then added into mixed system again, stirring is extremely
It is completely dissolved, obtains solution B；
(3) solution A is added in solution B, adds sodium chloride, after stirring, add sodium hydroxide and sodium acid carbonate
Mixed solution, adjust pH to 10.8, be then placed in ice-water bath；
(4) 0.5mol/L NaHB solution is added dropwise into the mixed system of step (3), and system is slowly stirred, drips
After adding end, mixed solution is warming up to 50 DEG C, and is incubated 72h, obtains granular disintegration；
(5) after granular disintegration is cleaned with saturated sodium-chloride, then cleaned with ethanol, particle diameter is obtained after vacuum drying is
The mol ratio of 18nm platinum-nickel alloy, wherein platinum and nickel is 4:1.
Embodiment 4：
A kind of preparation method of Platinum Nanoparticles nickel alloy catalyst for direct methanol dye cell, comprises the following steps：
(1) 0.2mmol TBABs are dissolved in 20mL isopropanols, obtain solution A；
(2) 1g chloroplatinic acids are dissolved in 100mL water, the chloroplatinic acid aqueous solution that concentration is 0.0193mol/L are obtained, then to it
Middle addition 2.5mL 0.1mol/L nickel chloride aqueous solutions, 8g PVP (Mw=40000), stirring are then added into mixed system again
To being completely dissolved, solution B is obtained；
(3) solution A is added in solution B, adds sodium chloride, after stirring, added sodium hydroxide solution, adjust pH
To 9, then it is placed in ice-water bath；
(4) 0.5mol/L NaHB solution is added dropwise into the mixed system of step (3), and system is slowly stirred, drips
After adding end, mixed solution is warming up to 50 DEG C, and is incubated 48h, obtains granular disintegration；
(5) after granular disintegration is cleaned with saturated sodium-chloride, then cleaned with ethanol, particle diameter is obtained after vacuum drying is
The mol ratio of 20nm platinum-nickel alloy, wherein platinum and nickel is 5:1.
To sum up, the embodiment of the present invention has the advantages that：The present invention makees due to the collaboration between metal platinum and metallic nickel
With improving the activity and electrocatalysis characteristic of metal, reduce the usage amount of noble metal platinum, reduce cost, and platinum nickel closes
Gold utensil has homogeneous size and institutional framework, and larger specific surface area, and further increasing methanol catalytic oxidation has significantly
Effect, and the preparation method of platinum-nickel alloy is simple, gentle controllable, it is not necessary to too high temperature and harsh experiment condition, it is real
Test stablize, yield it is high.
It should be noted that herein, such as first and second or the like relational terms are used merely to a reality
Body or operation make a distinction with another entity or operation, and not necessarily require or imply and deposited between these entities or operation
In any this actual relation or order.Moreover, term " comprising ", "comprising" or its any other variant are intended to
Nonexcludability includes, so that process, method, article or equipment including a series of elements not only will including those
Element, but also the other element including being not expressly set out, or it is this process, method, article or equipment also to include
Intrinsic key element.In the absence of more restrictions, the key element limited by sentence "including a ...", it is not excluded that
Other identical element also be present in process, method, article or equipment including the key element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
The present invention is described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic；And these modification or
Replace, the essence of appropriate technical solution is departed from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (8)
1. the preparation method of a kind of nanometer of platinum-nickel alloy, it is characterised in that comprise the following steps：
(1) surfactant is dissolved in organic solution, obtains solution A；
(2) 1g chloroplatinic acids are dissolved in 100mL water, then add 2~5mL0.1mol/L nickel chloride aqueous solutions thereto, then
5~8g PVP are added into mixed system again, stirs to being completely dissolved, obtains solution B；
(3) solution A is added in solution B, adds sodium chloride, after stirring, added alkaline solution, adjust pH to 9~12,
Then it is placed in ice-water bath；
(4) 0.5mol/LNaBH is added dropwise into the mixed system of step (3)4Solution, and system is slowly stirred, knot is added dropwise
Shu Hou, mixed solution is warming up to 50~70 DEG C, and is incubated 24~72h, obtain granular disintegration；
(5) after granular disintegration is cleaned with saturated sodium-chloride, then cleaned with ethanol, the conjunction of Platinum Nanoparticles nickel is obtained after vacuum drying
Gold.
2. the preparation method of as claimed in claim 1 nanometer of platinum-nickel alloy, it is characterised in that the organic solvent be ethanol,
One kind in ethylene glycol, isopropanol.
3. the preparation method of as claimed in claim 2 nanometer of platinum-nickel alloy, it is characterised in that the surfactant is 16
One kind in alkyl trimethyl ammonium bromide, tetrabutyl phosphonium bromide phosphine, TBAB.
4. the preparation method of as claimed in claim 3 nanometer of platinum-nickel alloy, it is characterised in that the surfactant solution
Concentration is 0.01~0.05mol/L.
5. the preparation method of as claimed in claim 4 nanometer of platinum-nickel alloy, it is characterised in that the mean molecule quantity of the PVP
For 40000.
6. the preparation method of as claimed in claim 5 nanometer of platinum-nickel alloy, it is characterised in that the alkaline solution is hydroxide
One or more compositions in sodium solution, sodium carbonate liquor, sodium bicarbonate solution.
7. a kind of nanometer platinum-nickel alloy prepared such as any methods described of claim 1~6, it is characterised in that Platinum Nanoparticles nickel closes
The mol ratio of platinum and nickel is 4~10 in gold:1, its alloying pellet particle diameter is 10~20nm.
8. a kind of application of nanometer platinum-nickel alloy as claimed in claim 7, it is characterised in that the nanometer platinum-nickel alloy can use
In the catalyst of methanol fuel cell.
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| CN108786845A (en) * | 2018-06-27 | 2018-11-13 | 济南大学 | A kind of preparation method of dendroid Pt-Ni-Cu alloy nanoparticles |
| CN110788345A (en) * | 2018-08-01 | 2020-02-14 | 中国科学院大连化学物理研究所 | Size-controllable Pt1Ag28Synthesis method of alloy nanocluster |
| CN109604628B (en) * | 2019-02-01 | 2021-12-24 | 东南大学 | Preparation method of ordered phase iron platinum nano-particles and cobalt platinum nano-particles |
| CN111715236B (en) * | 2020-06-02 | 2023-11-24 | 孙黎明 | Preparation method of multilayer nanoscale platinum-nickel alloy nano dendrite material |
| CN113070059A (en) * | 2021-03-25 | 2021-07-06 | 湘潭银河新能源有限公司 | Preparation method of platinum-based composite nano electrode catalyst |
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| CN101817088B (en) * | 2009-02-27 | 2011-12-28 | 天津商业大学 | Preparation method of Pt-Ni alloy nano particle and colloidal dispersion system thereof |
| CN102179525B (en) * | 2011-04-15 | 2013-05-08 | 北京航空航天大学 | Controllable synthesis method for preparing nickel platinum double-layered nanometer bowl at room temperature |
| CN103192086B (en) * | 2012-01-10 | 2015-05-13 | 中国科学院宁波材料技术与工程研究所 | Preparation method for controllable duplex metal alloy nano particle |
| CN103157494A (en) * | 2013-04-01 | 2013-06-19 | 河北师范大学 | Method of synthesizing Pt-Ni catalyst material by hydrothermal method |
| CN104096575A (en) * | 2014-06-26 | 2014-10-15 | 南京航空航天大学 | Method for preparing platinum-nickel nucleocapsid structure fuel cell catalyst through microwave reduction |
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