CN113862694B - Iron-doped nickel phosphide nano-particle and preparation method thereof - Google Patents
Iron-doped nickel phosphide nano-particle and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an iron-doped nickel phosphide nanoparticle and a preparation method thereof, comprising the following steps: (1) Putting ferric nitrate, nickel nitrate, terephthalic acid and carbon nano tube slurry into 40 ml of N, N-dimethylformamide and 16 ml of ethanol, and magnetically stirring for 30 minutes; (2) Pouring the liquid into a 100 milliliter inner container of a hydrothermal reaction kettle; (3) Putting the hydrothermal reaction kettle into an oven, setting the temperature and the heat preservation time, and cooling to the room temperature; (4) Centrifuging, washing the product with water and ethanol, and drying. (5) And (3) putting a certain amount of precursor and sodium hypophosphite at two ends of a quartz boat, putting the quartz boat into a tube furnace, introducing gas, setting the temperature and the heating rate, and cooling to room temperature to obtain the iron-doped nickel phosphide nano particles. The iron-doped nickel phosphide prepared by the method has large specific surface area and more active sites, is simple to operate and good in repeatability, can be prepared on a large scale, and provides a reliable sample preparation method for the application of phosphide in the aspect of water electrolysis.
Description
Technical Field
The invention belongs to the field of preparation of novel organic porous nano materials, and in particular relates to a method for preparing iron-doped nickel phosphide nano particles.
Background
Recently, the technology of water electrolysis is environment-friendly and can continuously produce hydrogen in a large scale, so that the technology is used as a promising method and attracts the interests of vast researchers. Meanwhile, the development of the electrocatalyst is closely related to the high-efficiency electrolysis of water. Currently, the most excellent HER catalyst is Pt/C and OER catalyst is IrO 2 And RuO (Ruo) 2 However, their scarcity and expensive cost limit the practical use of large-scale hydrogen production. The transition metal phosphide has the characteristics of low cost, high activity and durable stability, and is suitable for high-efficiency electrolysis of water in alkaline environment. Recently, researchers have found a new transition metal phosphide-iron doped nickel phosphide, the morphology of which presents the shape of a nanosheet, which is composed of a plurality of nanoparticles, the size of the nanoparticles being about 13 nanometers, the voids between the nanoparticles exposing a considerable active specific surface area, which is beneficial to promoting the smooth progress of the electrochemical reaction. At present, methods for preparing phosphide mainly comprise a hydrothermal method, an electrochemical deposition method and an impregnation method. The impregnation method mainly comprises the steps of mixing various raw materials and a solvent together, fully stirring, and standing for a period of time. This method requires a strict control of the time, since the material is greatly affected by the time during nucleation or growth. In addition, the morphology of the material is difficult to control without certain temperature and pressure treatment, which is unfavorable for the efficient preparation of the electrocatalyst.
The electrochemical deposition method mainly adopts a material with good electric conductivity as a substrate, such as: nickel foam, copper foam, carbon cloth, etc., and then improving the morphology and catalytic performance of the catalyst by adjusting the electrodeposition time. However, during practical operation, it is difficult to clarify the deposited potential and time, resulting in a great deal of time and waste of material. In order to solve the problems, the invention provides a hydrothermal reaction method, which takes ferric nitrate, nickel nitrate, terephthalic acid and carbon nano tube slurry raw materials, N, N-dimethylformamide and ethanol as solvents, and prepares the iron-doped nickel phosphide nano particles through the hydrothermal reaction and low-temperature phosphating. The invention has simple operation and can prepare high-quality electrocatalyst in large batch; in addition, the invention has high efficiency, good repeatability, simple control and low cost, and provides a reliable sample preparation method for the application of the iron-doped nickel phosphide in the aspect of water electrolysis.
Disclosure of Invention
In view of the above-described drawbacks of the prior art, an object of the present invention is to provide a method capable of simply, efficiently and easily preparing iron-doped nickel phosphide nanoparticles in a large scale, and the obtained iron-doped nickel phosphide nanoparticles.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a method for preparing iron-doped nickel phosphide nanoparticles, comprising the steps of:
(1) Taking 0.4mmol of ferric nitrate, 1.2mmol of nickel nitrate, 1.6mmol of terephthalic acid and 1.12g of carbon nano tube slurry as raw materials, and 40 ml of N, N-dimethylformamide and 16 ml of ethanol as solvents, and completely dissolving the four raw materials into the solvents to form a uniform solution;
(2) Transferring the formed solution into a lining of a hydrothermal reaction kettle;
(3) Then placing the hydrothermal reaction kettle into an oven;
(4) Heating the oven from room temperature to a preset temperature, and then preserving heat for a period of time;
(5) After the reaction is finished, cooling the oven to room temperature; taking out the hydrothermal reaction kettle;
(6) The obtained product is cleaned by water and ethanol and dried to obtain a precursor,
(7) Then, a proper amount of precursor and sodium hypophosphite are respectively put into the downstream and upstream of the quartz boat;
(8) And (8) putting the quartz boat into a tube furnace, introducing gas, vacuumizing, introducing argon, setting the heating rate to the heating temperature, heating and preserving the temperature for a period of time, and cooling to room temperature to obtain the iron-doped nickel phosphide nano particles.
Preferably, the oven preset temperature in step (4) is 160 ℃, which is favorable for the formation and growth of the nanoplatelets.
Preferably, the heat-preserving time in the step (4) is 6 hours. The heat preservation time is too long, the structure of the nano-sheet is destroyed, and if the time is insufficient, the nano-sheet is difficult to form.
Preferably, in step (7), the precursor and sodium hypophosphite are mixed in a ratio of 1: the mass ratio of 10 was placed downstream and upstream of the quartz boat, respectively.
Preferably, in the step (6), the precursor is obtained after the drying treatment by alternately washing 3 times with water and ethanol.
Preferably, the heating rate of the tube furnace in the step (8) is 3 ℃/min, so that the precursor can fully react with phosphine gas released by sodium hypophosphite.
Preferably, the tube furnace temperature in step (8) is 400 ℃ and the time is too long, so that the structure of the nano particles is destroyed, and if the time is insufficient, the nano particles are difficult to form.
Preferably, the heat preservation time of the tube furnace in the step (8) is 2h.
The invention also provides the iron-doped nickel phosphide nano-particles obtained by the method.
As described above, the present invention has the following advantageous effects: the method of the invention utilizes a hydrothermal reaction technology to make several medicines undergo chemical reaction to form a nickel-iron MOF (metal organic framework), then utilizes a tubular furnace phosphating technology to change a precursor into phosphide, and finally forms the iron-doped nickel phosphide nano particles. The method is simple to operate and low in cost, and can prepare high-quality iron-doped nickel phosphide nano particles in a large scale; the method has the characteristics of simple operation, good controllability, good repeatability and large-scale preparation, and provides a reliable sample preparation method for the application of phosphide in the aspect of preparing oxygen by electrolyzing water.
Drawings
FIG. 1 is an X-ray diffraction pattern of iron-doped nickel phosphide nanoparticles prepared in accordance with the present invention;
FIG. 2 is a Raman spectrum diagram of the iron-doped nickel phosphide nanoparticles prepared by the present invention;
in fig. 3, (a) is a scanning electron microscope image of the iron-doped nickel phosphide nanoparticles prepared according to the present invention, and (b) and (c) are transmission electron microscope images; (b) The inter-lattice fringe spacing is 0.165nm, corresponding to the (311) crystal plane of nickel phosphide, and the inter-lattice fringe spacing is 0.209nm, corresponding to the (201) crystal plane of nickel phosphide.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
Examples
A method for preparing iron-doped nickel phosphide nanoparticles, comprising the steps of:
(1) Taking 0.4mmol of ferric nitrate, 1.2mmol of nickel nitrate, 1.6mmol of terephthalic acid and 1.12g of carbon nano tube slurry as raw materials, and 40 ml of N, N-dimethylformamide and 16 ml of ethanol as solvents, and completely dissolving the four raw materials into the solvents to form a uniform solution;
(2) Transferring the formed solution into a lining of a hydrothermal reaction kettle;
(3) Then placing the hydrothermal reaction kettle into an oven;
(4) Heating the oven from room temperature to a preset temperature, and then preserving heat for a period of time; the heat preservation time is 6h. The heat preservation time is too long, the structure of the nano-sheet is destroyed, and if the time is insufficient, the nano-sheet is difficult to form. The preset temperature of the oven is 160 ℃, so that the appearance can be controlled by a certain pressure.
(5) After the reaction is finished, cooling the oven to room temperature; taking out the hydrothermal reaction kettle;
(6) Washing with water and ethanol for 3 times alternately, cleaning the obtained product, drying to obtain precursor,
(7) Then, a proper amount of precursor and sodium hypophosphite are taken according to the following ratio of 1:10, respectively placing the mass ratio into the downstream and upstream of the quartz boat;
(8) And (3) putting the quartz boat into a tube furnace, introducing gas, vacuumizing, introducing argon, setting the heating rate to be 3 ℃/min, heating to the heating temperature of 400 ℃, preserving heat for 2 hours, cooling to the room temperature, and finally obtaining the iron-doped nickel phosphide nano particles. The heating rate is 3 ℃/min, so that the precursor can fully react with phosphine gas released by sodium hypophosphite. The tube furnace temperature is 400 ℃, the time is too long, the structure of the nano particles is destroyed, and if the time is insufficient, the nano particles are difficult to form.
The embodiment also provides the iron-doped nickel phosphide nano-particles obtained by the method.
Fig. 1 is an X-ray diffraction pattern of iron-doped nickel phosphide prepared according to the present invention, and it can be seen that the synthesized product corresponds to the standard PDF card of two kinds of nickel phosphide, and no generation of iron phosphide was observed, because the content of iron was small, and this was also confirmed by the element content characterization, indicating that the iron-doped nickel phosphide was successfully prepared.
FIG. 2 is a Raman spectrum of the iron-doped nickel phosphide prepared by the method of the present invention, which can be seen at 1360cm -1 And 1580cm -1 Two characteristic raman peaks of C appear.
FIG. 3 is a transmission electron micrograph of iron-doped nickel phosphide prepared according to the present invention, wherein the nanosheets of iron-doped nickel phosphide nanoparticles are clearly seen, (b) the lattice fringe spacing is 0.165nm, corresponding to the (311) crystal plane of nickel phosphide, and (c) the lattice fringe spacing is 0.209nm, corresponding to the (201) crystal plane of nickel phosphide.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims of this invention, which are within the skill of those skilled in the art, can be made without departing from the spirit and scope of the invention disclosed herein.
Claims (2)
1. A method for preparing iron-doped nickel phosphide nanoparticles, characterized by comprising the steps of:
(1) Taking 0.4mmol of ferric nitrate, 1.2mmol of nickel nitrate, 1.6mmol of terephthalic acid and 1.12g of carbon nano tube slurry as raw materials, and 40 ml of N, N-dimethylformamide and 16 ml of ethanol as solvents, and completely dissolving the four raw materials into the solvents to form a uniform solution;
(2) Transferring the formed solution into a lining of a hydrothermal reaction kettle;
(3) Then placing the hydrothermal reaction kettle into an oven;
(4) Heating the oven from room temperature to a preset temperature, and then preserving heat for a period of time;
(5) After the reaction is finished, cooling the oven to room temperature; taking out the hydrothermal reaction kettle;
(6) The obtained product is cleaned by water and ethanol and dried to obtain a precursor,
(7) Then, a proper amount of precursor and sodium hypophosphite are respectively put into the downstream and upstream of the quartz boat;
(8) Putting the quartz boat into a tube furnace, introducing gas, vacuumizing, introducing argon, setting the heating rate to the heating temperature, heating and preserving the heat for a period of time, and cooling to room temperature to obtain iron-doped nickel phosphide nano particles; the nickel phosphide comprises nickel phosphide and nickel phosphide;
the preset temperature of the oven in the step (4) is 160 ℃;
the heat preservation time in the step (4) is 6 hours;
in the step (6), water and ethanol are alternately used for washing for 3 times, and a precursor can be obtained after drying treatment;
in the step (7), the precursor and sodium hypophosphite are mixed according to the following ratio of 1:10 mass ratio is respectively placed at the downstream and upstream of the quartz boat;
the heating rate of the tube furnace in the step (8) is 3 ℃/min;
the temperature of the tube furnace in the step (8) is 400 ℃;
and (3) the heat preservation time of the tubular furnace in the step (8) is 2 hours.
2. Iron-doped nickel phosphide nanoparticles obtained by the process of claim 1.
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| KR102589924B1 (en) * | 2018-08-16 | 2023-10-17 | 현대자동차주식회사 | Method of manufacturing electrocatalyst through one step electrodeposition and manufactured electrocatalyst therefrom |
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