CN108247080B - Platinum-copper-nickel ternary alloy nano material and preparation method thereof - Google Patents
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Abstract
A platinum-copper-nickel ternary alloy nano material and a preparation method thereof relate to functional materials. The platinum-copper-nickel ternary alloy nano material consists of three metals, namely platinum, copper and nickel, wherein the ratio of Pt to Cu to Ni is 18: 4: 1, the overall particle size can be 2-30 nm, and the material is uniform in overall appearance, uniform in particle size and good in dispersibility. During preparation, preparing an inorganic platinum salt precursor, adding a mixed solution into the inorganic platinum salt precursor, mixing the mixed solution with a copper salt, a nickel salt, carbon black and a solvent, mixing the mixture with a reducing agent after ultrasonic dispersion, heating and stirring the mixture, and reacting the mixture to prepare a solution; and cooling the prepared solution, centrifugally settling, taking the precipitate, and washing to obtain the platinum-copper-nickel ternary alloy nano material. The reaction condition in the preparation process is mild, the repeatability is high, and the preparation method is environment-friendly; the prepared nano material has the advantages of high stability, high electrocatalytic activity, low cost and the like.
Description
Technical Field
The invention relates to a functional material, in particular to a platinum-copper-nickel ternary alloy nano material and a preparation method thereof.
Background
With the rapid development of economy and the continuous increase of fossil energy consumption, people are facing increasingly serious problems of energy shortage and environmental destruction. The method develops high-efficiency clean energy, gradually replaces the traditional fossil energy, and has important significance for guaranteeing energy safety, promoting environmental protection, reducing greenhouse gas emission and realizing national economy sustainable development. A fuel cell is a highly efficient, environmentally friendly power generation device that can directly convert chemical energy stored in a fuel and an oxidant into electrical energy. Today, where the environment and energy are receiving attention, there is a need for the vigorous development of fuel cell technology. Electrocatalysts are key materials of fuel cells, and to obtain high efficiency and high specific energy in fuel cell systems, the reactivity of fuel and oxidant in the electrode process must be improved, i.e. high-efficiency catalysts must be researched and developed. At present, the polymer electrolyte fuel cell generally uses noble metal platinum as the main component of the catalyst, but the cost of the polymer electrolyte fuel cell is high due to the shortage of platinum resources and high price; in addition, impurity gases present in fuel and air, such as carbon monoxide, sulfur oxides, nitrogen oxides, and the like, tend to cause cumulative effects of catalyst poisoning, which is one of the root causes of low life of fuel cells. The high cost and low service life severely limit the progress of commercialization of fuel cells. Therefore, how to increase the activity of the catalyst and reduce the amount of platinum used in the electrode has become an important issue in the field of fuel cell research.
The main research directions of the current catalyst are the following three types: (1) the alloy of platinum and other metals is synthesized, so that the dosage of the metal platinum is effectively reduced, and the catalytic activity of the catalyst is improved to a certain extent. PtRu developed by Li, Miaoyu et al has a much higher catalytic activity than platinum single crystal materials (Li M, Zheng H, Han G, et al. simple synthesis of binary Pteroflowers for advanced electrocatalysts heated metal oxidation [ J ]. Catalysis Communications,2017,92: 95-99.). (2) For example, patent CN105013479A discloses a nano material with a silver core/platinum shell structure and a preparation method thereof, and the catalytic activity of the catalyst is superior to that of a platinum single crystal material. (3) The non-platinum catalyst with high efficiency and low cost is developed to replace the platinum catalyst. In recent years, the activity and stability under acidic environment of non-platinum catalysts have been greatly improved, but there is still a great gap from platinum-based catalysts.
Disclosure of Invention
The invention aims to provide a platinum-copper-nickel ternary alloy nano material and a preparation method thereof.
The platinum-copper-nickel ternary alloy nano material consists of three metals, namely platinum, copper and nickel, wherein the ratio of Pt to Cu to Ni is 18: 4: 1, the overall particle size can be 2-30 nm, and the material is uniform in overall appearance, uniform in particle size and good in dispersibility.
The preparation method of the platinum-copper-nickel ternary alloy nano material comprises the following steps:
1) preparing an inorganic platinum salt precursor, adding a mixed solution into the inorganic platinum salt precursor, mixing the mixed solution with a copper salt, a nickel salt, carbon black and a solvent, mixing the mixture with a reducing agent after ultrasonic dispersion, heating and stirring the mixture, and reacting the mixture to prepare a solution;
2) cooling the solution prepared in the step 1), centrifuging, settling, taking the precipitate, and washing to obtain the platinum-copper-nickel ternary alloy nano material.
In step 1), the inorganic platinum salt precursor may be one selected from chloroplatinic acid, potassium tetrachloroplatinate, potassium hexachloroplatinate, platinum nitrate, etc.; the copper salt can be selected from one of copper nitrate, copper sulfate, copper chloride and the like; the nickel salt can be selected from one of nickel sulfate, nickel nitrate, nickel carbonate and the like; the solvent can be one selected from water, lower alcohol, lower ketone, etc.;
the molar ratio of the inorganic platinum salt precursor to the copper salt to the nickel salt can be 1: 1-8; the molar ratio of the carbon black to the inorganic platinum salt precursor may be (10: 1) to (1: 10).
The ultrasonic dispersion time can be 0.1-5 h;
the reducing agent can be selected from one of ascorbic acid, sodium sulfite, ethylene glycol and the like; the reaction temperature can be 60-150 ℃, and the reaction time can be 1-24 h.
In step 2), the washing may be 3 times with ethanol.
The nano material prepared by the invention is composed of three metals of platinum, copper and nickel, the whole grain diameter can be controlled between 2 nm and 30nm, the grain diameter is uniform, the whole appearance is uniform, and the dispersibility is good. The preparation method does not need to use a surfactant, has simple preparation process, convenient operation, mild reaction conditions in the preparation process, high repeatability and environmental friendliness; the prepared nano material has the advantages of high stability, high electrocatalytic activity, low cost and the like, and has important application value in the fields of electrochemical catalysis, chemical sensors, photocatalysis, chemical catalysis and the like.
Drawings
FIG. 1 is a transmission electron microscope image of the Pt-Cu-Ni ternary alloy nanomaterial prepared in example 1 at low magnification. In FIG. 1, the scale is 20 nm.
FIG. 2 is a transmission electron microscope image of the Pt-Cu-Ni ternary alloy nanomaterial prepared in example 2 at high magnification. In FIG. 2, the scale is 5 nm.
FIG. 3 is a TEM image of the ternary Pt-Cu-Ni alloy nanoparticles prepared in example 10. In FIG. 3, the scale is 50 nm.
Fig. 4 is an X-ray diffraction (XRD) pattern of the ternary platinum-copper-nickel alloy nanomaterial prepared in example 10 (in comparison with the binary platinum-copper alloy). In fig. 4, the abscissa is the double incident angle (2-Theta,2 θ) and the ordinate is the diffraction Intensity (Intensity), and fig. 4 shows a comparison of the platinum-copper-nickel ternary alloy material and the copper-platinum alloy material; curve a is PtCu and curve b is PtCuNi.
FIG. 5 is a TEM image of the ternary Pt-Cu-Ni alloy nanoparticles prepared in example 11. In FIG. 5, the scale is 10 nm.
Detailed Description
The following examples will further illustrate the present invention with reference to the accompanying drawings.
Example 1
Taking 0.140g of potassium tetrachloroplatinate, 0.085g of copper nitrate and 0.096g of nickel sulfate into a reagent bottle, adding a small amount of water, and performing ultrasonic dispersion for 6min until the solution is completely dissolved; and then 40ml of ethylene glycol is taken to be put into a round bottom flask, 0.2g of carbon black is added, ultrasonic dispersion is carried out for 6min, then the carbon black is uniformly dissolved into the ethylene glycol, then the inorganic salt solution in the reagent bottle is poured into the round bottom flask, heating is carried out for 24h at 100 ℃, finally cooling and centrifugal sedimentation are carried out, and the precipitate is taken and washed for 3 times by ethanol, thus obtaining the platinum-copper-nickel ternary alloy nano material. FIG. 1 shows a transmission electron microscope image of a Pt-Cu-Ni ternary alloy nanomaterial at low magnification, with a scale of 20 nm. As can be seen in FIG. 2, the alloy nano-catalyst has relatively uniform dispersion and uniform size.
Example 2
Taking 0.126g of chloroplatinic acid, 0.054g of copper chloride and 0.768g of nickel sulfate into a reagent bottle, adding a small amount of ethanol, and performing ultrasonic dispersion for 30min until the solution is completely dissolved; and adding 200ml of ethylene glycol into a round-bottom flask, adding 0.8g of carbon black, performing ultrasonic dispersion for 30min, uniformly dissolving the carbon black in the ethylene glycol, pouring an inorganic salt solution in a reagent bottle into the round-bottom flask, heating at 150 ℃ for 18h, finally cooling, performing centrifugal sedimentation, washing the precipitate with ethanol for 3 times, and thus obtaining the platinum-copper-nickel ternary alloy nano material. FIG. 2 shows a transmission electron microscope image of a platinum-copper-nickel ternary alloy nanomaterial at high magnification, with a ruler of 5 nm. As can be seen from FIG. 2, the alloy nano-catalyst has good dispersibility and uniform size.
Example 3
Similar to example 1, except that 0.166g of potassium hexachloroplatinate was used as the inorganic platinum salt precursor, the same results as in example 1 were obtained.
Example 4
Similar to example 1, except that 0.120g of platinum nitrate was used as the inorganic platinum salt precursor, the same results as in example 1 were obtained.
Example 5
Similar to example 1, except that 0.092g of copper sulfate was used as the copper salt, the same results as in example 1 were obtained.
Example 6
Similar to example 1, except that 0.085g of nickel nitrate was used as the nickel salt, the same results as in example 1 were obtained.
Example 7
Similar to example 1, except that 0.082g of nickel carbonate was used as the nickel salt, the same result as in example 1 was obtained.
Example 8
Similar to example 2, except that 40ml of freshly prepared 0.6M sodium sulfite solution was used as the reducing agent, the same results as in example 2 were obtained.
Example 9
Similar to example 2, except that 40ml of freshly prepared 0.6M ascorbic acid solution was used as the reducing agent, the same results as in example 2 were obtained.
Example 10
Taking 0.140g of potassium tetrachloroplatinate, 0.085g of copper nitrate and 0.096g of nickel sulfate into a reagent bottle, adding a small amount of propanol, and performing ultrasonic dispersion for 1 hour until the solution is completely dissolved; and then 40ml of ethylene glycol is taken to be put into a round bottom flask, 0.2g of carbon black is added, ultrasonic dispersion is carried out for 1h, then the carbon black is uniformly dissolved into the ethylene glycol, then the inorganic salt solution in the reagent bottle is poured into the round bottom flask, heating is carried out for 24h at 100 ℃, finally cooling and centrifugal sedimentation are carried out, and the precipitate is taken and washed for 3 times, so that the platinum-copper-nickel ternary alloy nano material is obtained, and the obtained result is the same as that of the example 2. FIG. 3 shows a transmission electron microscope image of a Pt-Cu-Ni ternary alloy nanomaterial at low magnification, with a scale of 50 nm. As can be seen from FIG. 3, the alloy nano-catalyst has good dispersibility and uniform size. Fig. 4 shows an X-ray diffraction (XRD) pattern of the prepared pt-cu-ni ternary alloy nanomaterial, in comparison with a pt-cu binary alloy. The abscissa is the double incident angle (2-Theta,2 Theta) and the ordinate is the diffraction Intensity (Intensity), and it can be found from fig. 4 that the diffraction peaks of the metal platinum of the alloy nano material are shifted to the right to some extent compared with the elemental metal platinum, which is caused by the doping of the copper atoms and the nickel atoms.
Example 11
Taking 0.140g of potassium tetrachloroplatinate, 0.085g of copper nitrate and 0.096g of nickel sulfate into a reagent bottle, adding a small amount of ethanol, and performing ultrasonic dispersion for 5 hours until the solution is completely dissolved; and then 40ml of ethylene glycol is taken to be put into a round bottom flask, 1.0g of carbon black is added, ultrasonic dispersion is carried out for 5 hours, the carbon black is uniformly dissolved into the ethylene glycol, then the inorganic salt solution in the reagent bottle is poured into the round bottom flask, heating is carried out for 12 hours at the temperature of 100 ℃, then cooling and centrifugal sedimentation are carried out, and the precipitate is taken and washed for 3 times, so that the platinum-copper-nickel ternary alloy nano material is obtained, and the obtained result is the same as that of the example 2. FIG. 5 shows a transmission electron microscope image of a platinum-copper-nickel ternary alloy nanomaterial at low magnification, with a ruler of 10 nm. As can be seen from fig. 5, the alloy nano-catalyst has good dispersibility and uniform size.
Example 12
Taking 0.140g of potassium tetrachloroplatinate, 0.085g of copper nitrate and 0.096g of nickel sulfate into a reagent bottle, adding a small amount of propanol, and performing ultrasonic dispersion for 1 hour until the solution is completely dissolved; and then 40ml of ethylene glycol is taken to be put into a round bottom flask, 2.0g of carbon black is added, ultrasonic dispersion is carried out for 1h, the carbon black is uniformly dissolved into the ethylene glycol, then the inorganic salt solution in the reagent bottle is poured into the round bottom flask, heating is carried out for 24h at 120 ℃, finally cooling and centrifugal sedimentation are carried out, and the precipitate is taken and washed for 3 times, so that the platinum-copper-nickel ternary alloy nano material is obtained, and the obtained result is the same as that of the example 2.
Claims (2)
1. A platinum-copper-nickel ternary alloy nano material is characterized by consisting of three metals of platinum, copper and nickel, wherein the ratio of Pt to Cu to Ni is 18: 4: 1 by mole ratio; the particle size of the platinum-copper-nickel ternary alloy nano material is 2-30 nm;
the preparation method of the platinum-copper-nickel ternary alloy nano material comprises the following steps:
1) preparing an inorganic platinum salt precursor, adding a mixed solution into the inorganic platinum salt precursor, mixing the mixed solution with a copper salt, a nickel salt, carbon black and a solvent, mixing the mixture with a reducing agent after ultrasonic dispersion, heating and stirring the mixture, and reacting the mixture to prepare a solution; the molar ratio of the inorganic platinum salt precursor to the copper salt to the nickel salt is 1: 1-8; the molar ratio of the carbon black to the inorganic platinum salt precursor is (10: 1) to (1: 10); the inorganic platinum salt precursor is selected from one of chloroplatinic acid, potassium tetrachloroplatinate, potassium hexachloroplatinate and platinum nitrate; the copper salt is selected from one of copper nitrate, copper sulfate and copper chloride; the nickel salt is selected from one of nickel sulfate, nickel nitrate and nickel carbonate; the solvent is selected from one of water, lower alcohol and lower ketone; the ultrasonic dispersion time is 0.1-5 h; the reducing agent is selected from one of ascorbic acid, sodium sulfite and ethylene glycol; the reaction temperature is 60-150 ℃, and the reaction time is 1-24 h;
2) cooling the solution prepared in the step 1), centrifuging, settling, taking the precipitate, and washing to obtain the platinum-copper-nickel ternary alloy nano material.
2. The platinum-copper-nickel ternary alloy nanomaterial as defined in claim 1, wherein in the step 2), the washing is performed 3 times by using ethanol.
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| CN111437827B (en) * | 2019-01-17 | 2023-04-25 | 中国石油天然气股份有限公司 | Hollow ternary platinum nickel copper metal nanoparticle with surface capable of penetrating through platinum nickel copper, preparation and application |
| CN110165233A (en) * | 2019-05-27 | 2019-08-23 | 苏州氢极能源科技有限公司 | Catalyst of fuel batter with proton exchange film and preparation method thereof |
| CN111644635A (en) * | 2020-06-02 | 2020-09-11 | 孙黎明 | Preparation method of highly-recessed nanoscale platinum-copper-nickel alloy frame material |
| CN115156546B (en) * | 2021-03-19 | 2024-08-06 | 北京化工大学 | Preparation method of monodisperse PtM alloy nano particles or nanoclusters |
| CN113611877A (en) * | 2021-09-06 | 2021-11-05 | 无锡威孚高科技集团股份有限公司 | Multi-element alloy catalyst and preparation method and application thereof |
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