Preparation method of high dispersity Pt-Cu alloy nano-particles

A technology of alloy nanoparticles and high dispersibility, applied in nanotechnology, electrodes, electrolysis process, etc., can solve the problems of high cost of oleylamine and tetradecanediol, inability to obtain the target product in one step, and affecting the application performance of materials. , to achieve the effect of easy operation, easy industrial production and short reaction time

Active Publication Date: 2019-01-01
HARBIN UNIV OF SCI & TECH
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Problems solved by technology

[0006] The disadvantages are: 1) Cu seed crystals need to be prepared first, and the target product cannot be obtained in one step, and the reaction time is longer (more than 4 hours); 2) Oleylamine itself is expensive and has certain toxicity, and large-scale preparation will cause environmental damage. must destroy
[0008] Although this method achieves one-step preparation, it also has its inherent disadvantages: 1) First, since Cu is a transition metal, its reduction potential is much lower than that of Pt. In order to ensure the formation of alloys, the preparation needs to be carried out under high temperature reaction conditions; 2 ) Secondly, the cost and price of oleylamine and tetradecanediol are high during the preparation process, which is not suitable for large-scale production; 3) The organic ligands adsorbed on the surface are difficult to remove by simple cleaning, which directly affects the application performance of the material

Method used

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  • Preparation method of high dispersity Pt-Cu alloy nano-particles
  • Preparation method of high dispersity Pt-Cu alloy nano-particles
  • Preparation method of high dispersity Pt-Cu alloy nano-particles

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Embodiment 1: Preparation 1 of Pt-Cu alloy

[0040] With deionized water as the solvent and copper chloride as the solute, configure 7.5 ml of copper chloride solution with a concentration of 15 mmol / L; add 0.5 g of cetyltrimethylammonium chloride, and place in a constant temperature water bath at 95 degrees Celsius to evenly Stir; inject ascorbic acid solution with a volume of 2.5 ml and a concentration of 1.0 mol / L; when the solution turns from blue to transparent, add chloroplatinic acid with a volume of 1 ml and a concentration of 10 mmol / L, stir and heat for 20 minutes. The obtained product is separated by a centrifuge, dispersed in deionized water for ultrasonication, secondly centrifuged, dispersed in ethanol, and placed in a blast drying oven at 50 degrees after being centrifuged again for drying.

[0041] We first performed an X-ray diffraction test on the sample. from figure 1 It can be seen that the diffraction peaks of the obtained product are located betw...

Embodiment 2

[0045] Example 2: Verification of the effect of cetyltrimethylammonium chloride.

[0046] In order to verify the effect of adding cetyltrimethylammonium chloride in the whole preparation, we implement the following experiments: the operation in Example 1 "adding 0.5 gram of cetyltrimethylammonium chloride" is removed, and other conditions constant.

[0047] pass Figure 7 The X-ray diffraction pattern characterization we can obtain, the product of embodiment 2 is Cu 3 Pt and Cu 2 O complex. Field emission scanning electron microscopy results can be seen: the complex is granular, with a particle size of 0.5 to 1.2 microns (see Figure 8 ). This example proves that without the participation of cetyltrimethylammonium chloride, the reduction of divalent Cu ions is too fast, and some of the divalent Cu ions remain in Cu without being reduced to elemental Cu. 2 In the O stage, alloys with higher purity cannot be produced. Example 2 proves to us that the addition of cetyltrime...

Embodiment 3

[0048] Embodiment 3: the effect verification of chloroplatinic acid

[0049] In order to verify the effect of chloroplatinic acid in the preparation of Pt-Cu alloys, we implement the following experiments: in Example 1, "the solution is to be changed from blue to transparent, add 1 milliliter, and the concentration is 10 mmol / liter of platinum chloride Acid" step is deleted, and other operations remain unchanged. The results showed that no precipitated product was produced after 20 minutes or even longer reaction time. This example proves that ascorbic acid cannot reduce the divalent Cu source to elemental Cu with the participation of chlorine-free platinum acid. Example 3 proves to us that chloroplatinic acid plays the role of providing Pt source and promoting the conversion of divalent Cu to zero-valent Cu in the reaction.

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Abstract

The invention provides a preparation method of a high dispersity Pt-Cu alloy nano-particles, and belongs to the technical field of alloy nanometer material preparation. The preparation process comprises the following steps that a precursor copper chloride solution is prepared, heating and stirring are carried out at 90-100 DEG C, long-chain alkylamine is added, reducing agent ascorbic acid is added, chloroplatinic acid, and then heating is carried out for 20-30 minutes. In the preparation process, the addition of the long-chain alkylamine can improve the single dispersity of the Pt-Cu alloy nano-particles, and through the reducing of the reaction rate, the generation of impurity phases is inhibited. The chloroplatinic acid plays a role in providing a Pt source and promoting the conversionof divalent Cu into zero valence Cu in the reaction. According to the preparation method, the operation is simple, the method is green and environment-friendly, the production cost is low, and the preparation environment is easy to implement. The prepared Pt-Cu alloy has high dispersity and surface cleanness. In the catalytic application of the hydrogen evolution reaction, the Pt-Cu alloy has excellent catalytic stability performance.

Description

technical field [0001] The invention belongs to the technical field of nanoparticle preparation, and in particular relates to a simple method for preparing Pt-Cu alloy nanoparticle with high dispersibility by means of "hydrothermal reduction". Background technique [0002] In recent years, due to the development and use of traditional fossil energy, the air quality problem in northern my country has become increasingly serious. Air pollution and smog have seriously endangered public health. The development of new energy has gradually become an important way to solve environmental problems and promote green development. Among many new energy sources, hydrogen has long been considered as the most ideal clean energy due to its high energy density and zero emission of carbon dioxide after combustion. At present, water electrolysis is an important means of hydrogen production. However, in practice, the hydrogen production potential of electrolyzed water is much higher than the...

Claims

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Application Information

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IPC IPC(8): B22F9/24B82Y40/00C25B11/06C25B1/04
CPCC25B11/04B82Y40/00B22F9/24C25B11/097Y02E60/36
Inventor 刘欣美马艳斌杜杨韩睿泽隋永明邹勃
Owner HARBIN UNIV OF SCI & TECH
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