CN107919481B - Preparation method of 1nm ultrathin tube wall superfine single crystal platinum nanotube with openings at two ends - Google Patents
Preparation method of 1nm ultrathin tube wall superfine single crystal platinum nanotube with openings at two ends Download PDFInfo
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Abstract
A1 nm ultrathin tube wall with two open ends is a single crystal Pt nanotube with 5.5nm ultrathin diameter, 1nm ultrathin tube wall, tens of microns length and two open ends; the preparation method of the superfine single crystal platinum nanotube mainly comprises the steps of putting Pd nanowire powder and an ethylene glycol solution into a container, dropwise adding a chloroplatinic acid solution after stirring, carrying out centrifugal treatment after stirring, cleaning twice by using an ethanol-acetone solution, and drying to obtain Pd @ Pt core-shell structure nanowire powder; dissolving Pd @ Pt nanowire powder and ferric trichloride in a hydrochloric acid solution, magnetically stirring, centrifuging the mixed solution, and cleaning twice by using the hydrochloric acid solution to obtain the 1nm ultrathin single crystal platinum nanotube with the tube wall with openings at two ends. The preparation method is simple, and the prepared platinum nano tube has the advantages of superfine diameter, ultrathin tube wall, super length, single crystal structure, ultrahigh active specific surface area and high catalytic activity in the oxygen reduction reaction of the anode of the fuel cell.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a preparation method of a single crystal platinum nano material.
Technical Field
Energy is neither generated nor lost by the void, it can only be converted from one form to another. For example, in a fuel cell, chemical substances can convert chemical energy into electric energy in an efficient and environment-friendly manner through the action of a catalyst, and the fuel cell is the main content of the times of scientific research in environmental protection and energy conservation. The proton exchange membrane fuel cell has the characteristics of simple operation, mild reaction conditions, high power output, quick start and the like, and is widely applied to electric automobiles, electric motorcycles and portable power supply devices. In fuel cells, the reactions between the positive and negative electrodes require the participation of catalysts to work normally and efficiently, and thus, the preparation of catalysts necessary for electrode reactions is a hot spot of recent research. Among them, Pt has been used in production and life for a long time as the most efficient and stable catalyst. However, the most obstacle to putting such an environment-friendly and efficient power generation device into production on a larger scale and applying the device to the fields of transportation, industry, agriculture and the like is the limited and rare content of the precious metal catalyst Pt element in nature and the high price of the precious metal catalyst Pt element. Thus, in recent decades scientists have made extensive research efforts to synthesize efficient, small-sized, low Pt noble metal content catalysts.
Among them, the most common method for preparing a high-activity Pt catalyst is to minimize the size of the Pt nanomaterial and to increase the catalytic activity surface area of the Pt nanomaterial in a large range. For example, in 2012, the Gao topic group published in Journal of american chemical Society, and used insulin biological fiber as a biological template to prepare ultra-long Pt nanowires with a diameter of 1.8nm, both the catalytic activity surface area and the methanol oxidation efficiency were greatly improved. Subsequently, the journal of Nature materials reports that professor Nanfeng Zheng prepares the Pt nanowire with the diameter of only 1.1nm in a dimethylformamide solution by modifying and reducing ethylenediamine, and the ultrafine Pt nanowire has extremely high selective catalytic efficiency. Therefore, minimizing the size of the Pt nanomaterial is a common and effective means to increase its active surface area and thus catalytic activity.
In recent years, scientists have strived to increase the active surface area and also to decrease the amount of Pt used to increase the specific mass activity of noble metals by increasing the utilization of noble metals. The method is a method capable of simultaneously increasing the utilization rate of Pt surface atoms and reducing the platinum dosage. With the continuous development of research, scientists remove the core of the core-shell structure, so that the Pt atoms in the structure also participate in the catalytic reaction, the specific surface area of the structure becomes larger, and the utilization rate of Pt is improved to the greatest extent. The Pt nano tube is a typical nano material which can maximize the utilization rate of Pt nano particles and reduce the consumption of Pt element to the minimum.
In an early study on the preparation of Pt nanotubes, Yang topic group (angel. chem., int.ed.2007,46, 4060-. Recently, Haiwei, Liang et al (adv. Mater.2009,21, 1850-. Recently, Zhiqi Huang et al (J.Am.chem.Soc.2016,138,6332-6335) wrapped Pt element on the outer wall thereof using gold nanorods as the core, followed by Cu2+The Au nano-rod is etched by the etching method, so that a hollow Pt nano-tube polycrystalline structure with the diameter of 14-37nm and the wall thickness of 2-25nm is prepared, and the length of the hollow Pt nano-tube polycrystalline structure is only tens of nanometers. The preparation and research of the Pt nano-tubes by comprehensive scientists find that the synthesized Pt nano-tubes are mostly of polycrystalline irregular structures, the radius and the tube wall cannot reach the standard of minimum size at the same time, and most importantly, the hollow transparent structure with openings at two ends of the nano-tubes cannot be ensured.
Disclosure of Invention
The invention aims to provide a preparation method of a 1nm ultrathin tube wall double-end opening superfine single crystal platinum nanotube with superfine diameter, ultrathin tube wall, super length and single crystal structure.
The 1nm ultrathin tube wall two-end opening superfine single crystal platinum nanotube is a single crystal Pt nanotube which has the superfine diameter of 5.5nm, the ultrathin tube wall of 1nm, the length of tens of microns and is hollow and two-end opening.
The preparation method of the superfine single crystal platinum nanotube comprises the following steps:
(1) preparing a regular Pd @ Pt core-shell structure nanowire:
adding 0.1-1 mg of monocrystal Pd nanowire powder into per milliliter of ethylene glycol solution, putting the Pd nanowire powder with the diameter of 4.8nm and the ethylene glycol solution into a container, performing 50Hz ultrasonic treatment for 50-200 minutes to promote dissolution, then putting the mixed solution into a water bath, magnetically heating and stirring at the temperature of 50-80 ℃ for 10-40 minutes, controlling the stirring rate at 180-245 r/min, and then, adding the solution and the chloroplatinic acid solution according to the volume ratio of 15-40: 1, slowly dripping a chloroplatinic acid solution with the concentration of 3-8 mM into the mixed solution at the dripping speed of 0.75-2.5 mL/h, continuously heating and stirring at the temperature of 50-80 ℃ for 7-12 h, centrifuging the mixed solution for 15 minutes at 4000-9000 r/min, cleaning twice with an ethanol-acetone solution with the volume ratio of 2:1, and finally drying in a forced air drying box at 70 ℃ to obtain a large amount of regular Pd @ Pt core-shell structure nanowire powder;
(2) preparing single crystal Pt nanotubes:
adding 0.5-3 mg of Pd @ Pt nanowire powder and 0.2-0.8 mg of ferric chloride powder into a hydrochloric acid solution with the pH value of 1.5 per milliliter, uniformly dissolving the Pd @ Pt nanowire powder and the ferric chloride powder in the step (1) in the hydrochloric acid solution, putting the mixed solution into a container, carrying out magnetic heating and stirring for 0.5-2 hours at the temperature of 50-90 ℃, controlling the stirring rate at 150-250 r/min, centrifuging the mixed solution for 15 minutes at 3000-6000 r/min, and cleaning twice by using the hydrochloric acid solution with the pH value of 1.5 to obtain the ultrathin single crystal platinum nanotube with the ultrathin tube wall of 1nm and two open ends.
Compared with the prior art, the invention has the following advantages:
(1) the preparation method is simple, and the prepared platinum nano tube has an ultra-thin tube wall, an ultra-long length and a single crystal structure with ultra-thin diameter.
(2) The nano material has the characteristics of small size, hollowness and low Pt content, so the Pt nano tube has ultrahigh active specific surface area, shows high catalytic activity in the oxygen reduction reaction of the anode of the fuel cell and has outstanding superiority in the application aspect of the fuel cell.
Drawings
Figure 1 is a TEM image of a core template Pd nanowire used in example 1 of the present invention,
FIG. 2 is a TEM image of the ultra-fine and ultra-long Pd @ Pt core-shell structure nanowire prepared in example 2 of the present invention.
FIG. 3 is an HAADF-STEM diagram of the ultra-fine and ultra-long Pd @ Pt core-shell nanowire prepared in example 2 of the present invention (a)1) And line scan (a)2) And elemental analysis chart (a)3、a4)。
FIG. 4 is a TEM image of the ultra-fine and ultra-long single-crystal hollow Pt nanotube prepared in example 3 of the present invention.
FIG. 5 is a TEM image of the ultra-fine single-crystal Pt nanotube with two open ends prepared in example 4 of the present invention.
Example 1
(1) Putting 0.7mg of single crystal Pd nanowire powder with the diameter of 4.8nm and 1mL of glycol solution into a beaker, performing 50Hz ultrasonic treatment for 120 minutes to promote dissolution, then putting the mixed solution into a water bath, magnetically heating and stirring at 50 ℃ for 20 minutes, controlling the stirring rate at 245r/min, then slowly dropwise adding 2.5mL of chloroplatinic acid solution with the concentration of 6mM into the mixed solution at the dropwise adding speed of 2mL/h, continuously heating and stirring at 50 ℃ for 9 hours, then performing 6000r/min centrifugal treatment on the heated mixed solution for 15 minutes, cleaning twice by using ethanol-acetone solution with the volume ratio of 2:1, and finally drying in a blowing drying box at 70 ℃ to obtain a large amount of regular Pd @ Pt core-shell structure nanowire powder.
(2) And (2) putting 0.5mg of the Pd @ Pt nanowire powder prepared in the step (1) and 0.8mg of ferric trichloride powder into 1mL of hydrochloric acid solution with the pH value of 1.5 for uniform dissolution, putting the mixed solution into a beaker, carrying out magnetic heating and stirring for 0.5h at the temperature of 90 ℃, controlling the stirring rate at 250r/min, carrying out 6000r/min centrifugal treatment on the heated mixed solution for 15 min, and cleaning twice by hydrochloric acid with the pH value of 1.5 to obtain the superfine single crystal platinum nanotube with the two open ends of the ultrathin tube wall of 1 nm.
As shown in fig. 1, a in the figure shows that a large number of ultra-fine Pd nanowires have an ultra-long structure, and the length can reach tens of micrometers, and b in the figure shows that the ultra-fine Pd nanowires have a uniform radius (4.8nm) and a smooth surface.
Example 2
(1) Putting 0.2mg of single crystal Pd nanowire powder with the diameter of 4.8nm and 1mL of glycol solution into a beaker, performing 50Hz ultrasonic treatment for 70 minutes to promote dissolution, then putting the mixed solution into a water bath, magnetically heating and stirring the mixed solution at the temperature of 55 ℃ for 30 minutes, controlling the stirring rate at 220r/min, then slowly dripping 2mL of chloroplatinic acid solution with the concentration of 5mM into the mixed solution at the dripping speed of 1mL/h, continuously heating and stirring the mixed solution at the temperature of 55 ℃ for 10 hours, centrifuging the heated mixed solution for 15 minutes at 8000r/min, cleaning the mixed solution twice by using ethanol-acetone solution with the volume ratio of 2:1, and finally drying the mixed solution in a blast drying box at the temperature of 70 ℃ to obtain a large amount of regular Pd @ Pt core-shell structure nanowire powder.
(2) And (2) putting 1mg of the Pd @ Pt nanowire powder prepared in the step (1) and 0.5mg of ferric trichloride powder into 1mL of hydrochloric acid solution with the pH value of 1.5 for uniform dissolution, putting the mixed solution into a beaker, carrying out magnetic heating and stirring at the temperature of 70 ℃ for 1h, controlling the stirring rate at 220r/min, centrifuging the heated mixed solution for 15 minutes at 4000r/min, and cleaning twice by using hydrochloric acid with the pH value of 1.5 to obtain the 1nm ultrathin single crystal platinum nanotube with openings at two ends of the ultrathin tube wall.
As shown in FIG. 2, a shows that a large number of Pd @ Pt nanowires have a regular super-long structure, and b shows that the Pd @ Pt nanowires have a uniform radius of about 5.5 nm.
As shown in FIG. 3, a2Is corresponding to the drawing a1Linear profile at arrow from a2It can be seen that the Pt shell tube wall is about 1nm and the Pd core diameter is about 4.8 nm. a is3、a4In the elemental analysis chart, Pt is taken as a shell element, Pd is taken as a core element, and a uniform and regular core-shell structure is formed.
Example 3
(1) Putting 1mg of single crystal Pd nanowire powder with the diameter of 4.8nm and 1mL of glycol solution into a beaker, performing 50Hz ultrasonic (50Hz) for 200 minutes to promote dissolution, then putting the mixed solution into a water bath, magnetically heating and stirring the mixed solution at the temperature of 80 ℃ for 10 minutes, controlling the stirring rate at 180r/min, then slowly dripping 5mL of chloroplatinic acid solution with the concentration of 3mM into the mixed solution at the dripping speed of 2.5mL/h, continuously heating and stirring the mixed solution at the temperature of 80 ℃ for 12 hours, centrifuging the heated mixed solution for 15 minutes at 4000r/min, washing the mixed solution twice by using ethanol-acetone solution with the volume ratio of 2:1, and finally drying the mixed solution in a blast drying box at the temperature of 70 ℃ to obtain a large amount of regular Pd @ Pt core-shell structure nanowire powder.
(2) And (2) putting 3mg of the Pd @ Pt nanowire powder prepared in the step (1) and 0.3mg of ferric trichloride powder into 1mL of hydrochloric acid solution with the pH value of 1.5 for uniform dissolution, putting the mixed solution into a beaker, carrying out magnetic heating and stirring at the temperature of 50 ℃ for 2h, controlling the stirring rate at 150r/min, centrifuging the heated mixed solution for 15 min at 5000r/min, and cleaning twice by hydrochloric acid with the pH value of 1.5 to obtain the 1nm ultrathin single crystal platinum nanotube with the two open ends of the ultrathin tube wall.
As shown in fig. 4, a shows that the Pt nanotubes produced are abundant in yield, and b shows that a large number of Pt nanotubes have regular hollow tubular structures and the tube wall is about 1 nm.
Example 4
(1) Putting 0.1mg of single crystal Pd nanowire powder with the diameter of 4.8nm and 1mL of glycol solution into a beaker, performing 50Hz ultrasound (50Hz) for 50 minutes to promote dissolution, then putting the mixed solution into a water bath, magnetically heating and stirring the mixed solution at the temperature of 75 ℃ for 40 minutes, controlling the stirring rate at 200r/min, then slowly dripping 1mL of chloroplatinic acid solution with the concentration of 8mM into the mixed solution at the dripping speed of 0.75mL/h, continuously heating and stirring the mixed solution at the temperature of 75 ℃ for 7 hours, centrifuging the heated mixed solution for 15 minutes at 9000r/min, washing the mixed solution twice by using ethanol-acetone solution with the volume ratio of 2:1, and finally drying the mixed solution in a blast drying box at the temperature of 70 ℃ to obtain a large amount of regular Pd @ Pt core-shell structure nanowire powder.
(2) 2mg of the Pd @ Pt nanowire powder prepared in the step (1) and 0.2mg of ferric trichloride powder are put into 1mL of hydrochloric acid solution with the pH value of 1.5 to be uniformly dissolved, the mixed solution is put into a beaker, magnetic heating and stirring are carried out at the temperature of 60 ℃ for 1.5h, the stirring speed is controlled at 170r/min, then the heated mixed solution is subjected to centrifugal treatment at 3000r/min for 15 minutes, and hydrochloric acid with the pH value of 1.5 is used for cleaning twice, so that the superfine single crystal platinum nanotube with the two openings at the two ends of the ultrathin tube wall of 1nm is obtained.
As shown in FIG. 5, a, b and c can clearly see that the Pt nanotube has the characteristic of opening at two ends.
Claims (1)
1. A preparation method of a 1nm ultrathin tube wall superfine single crystal platinum nanotube with openings at two ends is characterized by comprising the following steps: the 1nm ultrathin tube wall superfine single crystal platinum nanotube with openings at two ends is a single crystal Pt nanotube which has the superfine diameter of 5.5nm, the ultrathin tube wall of 1nm and the length of tens of microns and is hollow and has openings at two ends, and the preparation steps are as follows:
(1) preparing a regular Pd @ Pt core-shell structure nanowire:
adding 0.1-1 mg of monocrystal Pd nanowire powder into per milliliter of ethylene glycol solution, putting the Pd nanowire powder with the diameter of 4.8nm and the ethylene glycol solution into a container, performing 50Hz ultrasonic treatment for 50-200 minutes to promote dissolution, then putting the mixed solution into a water bath, magnetically heating and stirring at the temperature of 50-80 ℃ for 10-40 minutes, controlling the stirring rate at 180-245 r/min, and then, adding the solution and the chloroplatinic acid solution according to the volume ratio of 15-40: 1, slowly dripping a chloroplatinic acid solution with the concentration of 3-8 mM into the mixed solution at the dripping speed of 0.75-2.5 mL/h, continuously heating and stirring at the temperature of 50-80 ℃ for 7-12 h, centrifuging the mixed solution for 15 minutes at 4000-9000 r/min, cleaning twice with an ethanol-acetone solution with the volume ratio of 2:1, and finally drying in a forced air drying box at 70 ℃ to obtain a large amount of regular Pd @ Pt core-shell structure nanowire powder;
(2) preparing single crystal Pt nanotubes:
adding 0.5-3 mg of Pd @ Pt nanowire powder and 0.2-0.8 mg of ferric chloride powder into a hydrochloric acid solution with the pH value of 1.5 per milliliter, uniformly dissolving the Pd @ Pt nanowire powder and the ferric chloride powder in the step (1) in the hydrochloric acid solution, putting the mixed solution into a container, carrying out magnetic heating and stirring for 0.5-2 hours at the temperature of 50-90 ℃, controlling the stirring rate at 150-250 r/min, centrifuging the mixed solution for 15 minutes at 3000-6000 r/min, and cleaning twice by using the hydrochloric acid solution with the pH value of 1.5 to obtain the ultrathin single crystal platinum nanotube with the ultrathin tube wall of 1nm and two open ends.
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