CN108658053B - Preparation method of loose structure CoP two-dimensional nanosheet - Google Patents
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Abstract
The invention discloses a preparation method of a loose structure CoP two-dimensional nanosheet, which comprises the steps of placing a cobalt hydroxide nanosheet serving as a precursor at one end of a porcelain boat, placing sodium metaphosphate at the other end of the porcelain boat, then placing the porcelain boat in a heating furnace protected by inert gas for heating reaction, wherein one end filled with the sodium metaphosphate faces to an air outlet of the heating furnace, and then sequentially washing, centrifugally collecting and drying products to obtain the loose structure CoP two-dimensional nanosheet. The invention adopts a high-temperature calcination method, and the preparation process is simple and easy to repeat. The CoP two-dimensional nanosheet has great application potential in the fields of capacitors, batteries, electrocatalysis and the like.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a preparation method of a loose-structure CoP two-dimensional nanosheet.
Background
The cobalt hydroxide has the characteristics of unique layered structure, excellent electrochemical performance, low cost and no pollution, and is a competitive electrode material in the fields of supercapacitors and electrocatalytic oxidation of water. However, as an electrocatalyst, cobalt hydroxide has poor conductivity and a large overpotential, and its application is widely limited.
Recently, phosphoric acid compounds and phosphorus compounds have been widely used as catalysts in the field of electrocatalytic oxidation of water. The load P on the two-dimensional layered double hydroxide nano-sheet can not only improve the conductivity of the material, but also increase the active area. Double metal hydroxides as H2Receiver, P as proton accepting center. P and the bimetallic compound play a synergistic role, so that the reaction activity can be improved. How to prepare the two-dimensional nanosheet with high electrocatalytic activity and stable crystal structure by a simple and feasible method is a technical problem which needs to be solved urgently.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a preparation method of a loose structure CoP two-dimensional nanosheet, and aims to prepare the two-dimensional nanosheet with excellent performance through a simple and easy method.
In order to achieve the purpose, the invention adopts the technical scheme that:
the preparation method comprises the steps of placing cobalt hydroxide nanosheets serving as precursors at one end of a porcelain boat, placing sodium metaphosphate at the other end of the porcelain boat, placing the porcelain boat in a heating furnace protected by inert gas for heating reaction, wherein one end filled with the sodium metaphosphate faces to an air outlet of the heating furnace, and then sequentially washing, centrifugally collecting and drying products to obtain the CoP two-dimensional nanosheets with loose structures.
Preferably, the precursor is prepared by the following method:
the preparation method of the precursor comprises the steps of adding ammonia water into a mixed solution of cobalt acetate and aluminum chloride, stirring for reaction, and then sequentially carrying out high-temperature reaction, centrifugal separation, washing and drying on the obtained precipitate to obtain Co (OH)2A two-dimensional nanoplate precursor; the reaction temperature of the high-temperature reaction is 110-130 ℃.
Preferably, the molar ratio of the cobalt acetate to the aluminium chloride solution is from 1 to 4:1, more preferably 2: 1. By adopting the proportion, the prepared precursor nanosheet is uniform in appearance and stable in crystal structure.
Preferably, the volume ratio of the solvent water to the ammonia water in the mixed solution of the cobalt acetate and the aluminum chloride is 5-15: 1. More preferably, the volume ratio is 10: 1. By adopting the proportion, the reaction can be fully performed to generate the precipitate. The mixed solution of cobalt acetate and aluminum chloride is obtained by dissolving cobalt acetate and aluminum chloride in distilled water and uniformly stirring; and the ammonia water is added into the uniformly mixed solution in a manner of adding the ammonia water while stirring for reaction by adding the ammonia water and stirring for 0.5 to 1 hour by magnetic force. Preferably, the stirring is magnetic stirring. Is convenient for being dispersed evenly.
The high-temperature reaction is carried out in a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining. Is convenient for the high-temperature reaction. And impurity elements are not mixed in the reaction process.
The washing is carried out by sequentially adopting distilled water and ethanol.
The drying is carried out by adopting an oven, the drying temperature is 60-80 ℃, and the drying time is 8-24 h.
The length of the cobalt hydroxide two-dimensional nano-sheet is 100-150nm, and the thickness is 2-5 nm.
Preferably, the mass ratio of the sodium metaphosphate to the precursor is 5-25: 1. More preferably, the mass ratio is 20: 1. Ensure that the precursor is just reacting completely.
Preferably, the heating furnace is a tube furnace, and the porcelain boat is a corundum porcelain boat. Inert gas is N2. The heating reaction is carried out at N2The temperature is raised to 350 ℃ at the heating rate of 2 ℃/min and is kept for 2 h.
And the washing of the product is sequentially carried out by adopting distilled water and ethanol, the drying is carried out by adopting an oven, the drying temperature is 60-80 ℃, and the drying time is 8-24 h.
The length of the CoP two-dimensional nanosheet is 100-150nm, and the thickness of the CoP two-dimensional nanosheet is 3-7 nm.
The invention has the beneficial effects that:
1) the high-temperature calcination method has simple preparation process and easy repetition.
2) The preparation method can obtain CoP, and the prepared loose structure CoP two-dimensional nanosheet is 150nm in length and 3-7nm in thickness.
3) With the precursor before phosphating (Co (OH)2) Compared with a loose structure CoP two-dimensional nanosheet, the CoP two-dimensional nanosheet has better electrocatalytic performance. Calculated available Co (OH)2With CoP at a current density of 10mA cm2The overpotential of (A) is 328mV and 483mV, respectively, and the Tafel slope is 109.72 and 274.67dec-1。
4) The loose-structure CoP two-dimensional nanosheet has great application potential in the fields of capacitors, batteries, electrocatalysis and the like.
Drawings
The description includes the following figures, the contents shown are respectively:
FIG. 1 shows the precursors (Co (OH) in example 12) XRD patterns of CoP two-dimensional nanosheet products of the product and the loose structure;
FIG. 2 is an SEM image; wherein a is the precursor (Co (OH) in example 12) SEM image of the product; b is the CoP two-dimensional sodium of the loose structure in example 1SEM images of rice flake products;
FIG. 3 is an SEM image; wherein a is the precursor (Co (OH) in example 22) SEM image of the product; b is an SEM image of a loose-structured CoP two-dimensional nanosheet product of example 2;
FIG. 4 is an SEM image; wherein a is the precursor (Co (OH) in example 32) SEM image of the product; b is an SEM image of a loose-structured CoP two-dimensional nanosheet product of example 3;
FIG. 5 is Co (OH)2Graph comparing linear voltammetry performance with CoP;
FIG. 6 is Co (OH)2Tafel slope comparison plot with CoP;
FIG. 7 is Co (OH)2Mass activity and TOF plots with CoP;
FIG. 8 is Co (OH)2Graph comparing impedance with CoP.
Detailed Description
The following detailed description of the embodiments of the present invention will be given with reference to the accompanying drawings for a purpose of helping those skilled in the art to more fully, accurately and deeply understand the concept and technical solution of the present invention and to facilitate its implementation.
The invention relates to a preparation method of a loose structure CoP two-dimensional nanosheet, which comprises the steps of placing a cobalt hydroxide nanosheet as a precursor at one end of a porcelain boat, placing sodium metaphosphate at the other end of the porcelain boat, then placing the porcelain boat in a heating furnace protected by inert gas for heating reaction, wherein one end filled with the sodium metaphosphate faces to an air outlet of the heating furnace, and then sequentially washing, centrifugally collecting and drying products to obtain the loose structure CoP two-dimensional nanosheet. The ratio of sodium metaphosphate to the precursor is 5-25: 1. The heating furnace preferably adopts a tube furnace, and the porcelain boat adopts a corundum porcelain boat. Inert gas is N2The heating reaction is carried out in N2The temperature is raised to 350 ℃ at the heating rate of 2 ℃/min and is kept for 2 h. Washing the product by sequentially adopting distilled water and ethanol, drying by adopting an oven at the temperature of 60-80 ℃ for 8-24 h.
The precursor is prepared by the following method:
the preparation method of the precursor comprises the steps of adding ammonia water into a mixed solution of cobalt acetate and aluminum chloride, stirring for reaction, and then sequentially carrying out high-temperature reaction, centrifugal separation, washing and drying on the obtained precipitate to obtain Co (OH)2A two-dimensional nanoplate precursor; the reaction temperature of the high-temperature reaction is 110-130 ℃. The molar ratio of the cobalt acetate to the aluminum chloride solution is 1-4: 1. The volume ratio of the solvent water to the ammonia water in the mixed solution of the cobalt acetate and the aluminum chloride is 5-15: 1. The mixed solution of cobalt acetate and aluminum chloride is obtained by dissolving cobalt acetate and aluminum chloride in distilled water and uniformly stirring; adding ammonia water and stirring for reaction, namely adding the ammonia water into the uniformly mixed solution in a manner of adding the ammonia water while stirring, and magnetically stirring for 0.5-1 h. The high temperature reaction is carried out in a stainless steel high pressure reaction kettle with a polytetrafluoroethylene lining. Is convenient for the high-temperature reaction. And impurity elements are not mixed in the reaction process. The washing is carried out by sequentially adopting distilled water and ethanol. Drying in an oven at 60-80 deg.C for 8-24 h. The cobalt hydroxide two-dimensional nano-sheet prepared by the method has the length of 100-150nm and the thickness of 2-5 nm. The precursor prepared by the method is applied to the loose-structure CoP two-dimensional nanosheet prepared by the preparation method, the crystal structure is more stable, and the loose-structure CoP two-dimensional nanosheet has better electrocatalytic performance.
The following is a detailed description of preferred embodiments:
example 1
A preparation method of a CoP two-dimensional nanosheet with a loose structure comprises the following steps:
(1) precursor (Co (OH)2) Preparation of
1) Adding 1mmol of cobalt acetate and 0.5mmol of aluminum chloride into 10mL of deionized water, uniformly stirring, then adding 1mL of ammonia water while stirring, and stirring for 0.5h by magnetic force to obtain a precipitate.
2) Pouring the precipitate into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, heating to 120 ℃, reacting for 2 hours, and cooling after the reaction is finished;
3) the reaction product is centrifugally separated, and then,obtaining solid powder, washing with distilled water and ethanol in sequence, and drying at 60 deg.C for 24 hr to obtain precursor (Co (OH)2) Two-dimensional nanosheets.
(2) Preparation of loose-structure CoP two-dimensional nanosheet
1) 0.05g Co (OH) is weighed out2The mixture was placed at one end of a corundum porcelain boat, and then 0.6g of sodium metaphosphate was weighed at the other end of the corundum porcelain boat. Placing the porcelain boat in N2Heating to 320 ℃ for 2h (one end filled with sodium metaphosphate faces to an air outlet) by a protected tube furnace at a temperature of 2 ℃/min, and cooling after the reaction is finished;
2) washing the reaction product with distilled water and ethanol in sequence, centrifuging, collecting, and drying at 60 ℃ for 24h to obtain the loose-structure CoP two-dimensional nanosheet.
The prepared precursor (Co (OH) was subjected to X-ray diffraction (XRD) and field emission scanning electron microscope (FE-SEM)2) And analyzing the CoP two-dimensional nanosheet product with a loose structure.
As shown in FIG. 1, the precursor (Co (OH))2) The XRD pattern of the product shows that all diffraction peaks are in the same layer form as standard α -Co (OH)2(card number: PDF # 46-0605). Peaks at diffraction angles (2 θ) of 11.543, 23.205, and 34.466 ° respectively correspond to the (003), (006), and (102) planes, respectively. From the XRD pattern of the loose-structure CoP two-dimensional nanosheet product, all diffraction peaks correspond to the crystal spectrogram of standard CoP (card number: PDF # 65-1474). Peaks at diffraction angles (2 θ) of 31.60, 35.33, 48.41, 56.01 and 59.90 ° respectively correspond to the (011), (200), (211), (020) and (113) crystal planes. The results show that the product of this example is CoP.
As shown in FIG. 2, a is the precursor (Co (OH) in example 12) SEM image of the product, from which the precursor (Co (OH))2) The length of the nano-sheet is about 100-150nm, and the thickness is about 2-5 nm. b is an SEM image of the CoP two-dimensional nanosheet product with the loose structure in example 1, and the CoP two-dimensional nanosheet with the loose structure is about 100-150nm long and about 3-7nm thick.
Example 2
A preparation method of a CoP two-dimensional nanosheet with a loose structure comprises the following steps:
(1) precursor (Co (OH)2) Preparation of
1) Adding 1mmol of cobalt acetate and 0.5mmol of aluminum chloride into 10mL of deionized water, uniformly stirring, then adding 1.25mL of ammonia water while stirring, and stirring for 0.5h by magnetic force to obtain a precipitate.
2) Pouring the precipitate into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, heating to 120 ℃, reacting for 8 hours, and cooling after the reaction is finished;
3) centrifugally separating the reaction product to obtain solid powder, washing with distilled water and ethanol in sequence, and drying at 60 deg.C for 24 hr to obtain precursor (Co (OH)2) Two-dimensional nanosheets.
(2) Preparation of loose-structure CoP two-dimensional nanosheet
1) 0.05g Co (OH) is weighed out2Placing the mixture in one end of a corundum porcelain boat, and weighing 1g of sodium metaphosphate to be placed in the other end of the corundum porcelain boat. Placing the porcelain boat in N2Heating to 320 ℃ for 2h (one end filled with sodium metaphosphate faces to an air outlet) by a protected tube furnace at a temperature of 2 ℃/min, and cooling after the reaction is finished;
2) washing the reaction product with distilled water and ethanol in sequence, centrifuging, collecting, and drying at 60 ℃ for 24h to obtain the loose-structure CoP two-dimensional nanosheet.
The prepared precursor (Co (OH) was aligned by field emission scanning electron microscope (FE-SEM)2) And analyzing the CoP two-dimensional nanosheet product with a loose structure.
As shown in FIG. 3, a is the precursor (Co (OH) in example 22) SEM image of the product, from which the precursor (Co (OH))2) The length of the nano-sheet is about 200-300nm, and the thickness is about 5-10 nm. b is an SEM image of the CoP two-dimensional nanosheet product with the loose structure in example 2, and the length of the CoP two-dimensional nanosheet with the loose structure is about 200-300nm and the thickness is 6-12 nm.
Example 3
A preparation method of a CoP two-dimensional nanosheet with a loose structure comprises the following steps:
(1) precursor (Co (OH)2) Preparation of
1) Adding 1mmol of cobalt acetate and 0.5mmol of aluminum chloride into 10mL of deionized water, uniformly stirring, then adding 0.86mL of ammonia water while stirring, and stirring for 0.5h by magnetic force to obtain a precipitate.
2) Pouring the precipitate into a stainless steel high-pressure reaction kettle with a polytetrafluoroethylene lining, heating to 120 ℃, reacting for 4 hours, and cooling after the reaction is finished;
3) centrifugally separating the reaction product to obtain solid powder, washing with distilled water and ethanol in sequence, and drying at 60 deg.C for 24 hr to obtain precursor (Co (OH)2) Two-dimensional nanosheets.
(2) Preparation of loose-structure CoP two-dimensional nanosheet
1) 0.05g Co (OH) is weighed out2The mixture was placed at one end of a corundum porcelain boat, and then 0.5g of sodium metaphosphate was weighed at the other end of the corundum porcelain boat. Placing the porcelain boat in N2Heating to 320 ℃ for 2h (one end filled with sodium metaphosphate faces to an air outlet) by a protected tube furnace at a temperature of 2 ℃/min, and cooling after the reaction is finished;
2) washing the reaction product with distilled water and ethanol in sequence, centrifuging, collecting, and drying at 60 ℃ for 24h to obtain the loose-structure CoP two-dimensional nanosheet.
The prepared precursor (Co (OH) was aligned by field emission scanning electron microscope (FE-SEM)2) And analyzing the CoP two-dimensional nanosheet product with a loose structure.
As shown in FIG. 4, a is the precursor (Co (OH) in example 32) SEM image of the product, from which the precursor (Co (OH))2) The length of the nano-sheet is about 150-250nm, and the thickness is about 3-7 nm. b is an SEM image of a loose-structured CoP two-dimensional nanosheet product of example 3, from which it can be seen that the loose-structured CoP two-dimensional nanosheets are about Xnm long and 5-10nm thick.
Example 4
Precursor (Co (OH) prepared in example 12) And testing the three-electrode electro-catalysis performance of the nano-sheet and the CoP two-dimensional nano-sheet with a loose structure. The method specifically comprises the following steps: separately, 4mg of Co (OH)2And CoP, adding 1.5mL of deionized water and 0.5mL of ethanol, performing ultrasonic treatment for about 1 hour, and then adding 45uL of Nafion conductive adhesive. And (4) transferring and dropping 15uL of the solution onto the pretreated glassy carbon electrode, and drying in an oven at the temperature of 60 ℃. After drying, electrochemical performance tests were performed using an electrochemical workstation (CHI 660E). The test is carried out in a three-electrode test system with 1mol/L KOH as electrolyte, a saturated Ag/AgCl electrode as a reference electrode and a platinum wire electrode as a counter electrode. The test result shows that: the CoP two-dimensional nanosheet with the loose structure has high electrocatalytic activity.
FIG. 5 is the precursor (Co (OH) prepared in example 12) And testing three-electrode electro-catalysis performance diagrams of the nano-sheet and the CoP two-dimensional nano-sheet with a loose structure. FIG. 5 shows Co (OH)2Graph comparing the linear voltammetric performance of CoP. From the figure, Co (OH) can be seen2The initial voltage of CoP was 1.4 and 1.51V, respectively, but the current density was 10mA cm2The initial voltage is 1.558V and 1.713V respectively, and the overpotential at the current density is 328mV and 483mV respectively through calculation. FIG. 6 shows Co (OH)2Tafel slope plot against CoP. The Tafel slope of CoP was 109.72dec-1Less than Co (OH)2Tafel slope 274.67dec-1. FIG. 7 shows Co (OH)2And mass activity and TOF plots of CoP. At a current density of 10mA cm2The mass activity and TOF values of CoP were 38.91A/g and 0.0094s, respectively-1，Co(OH)2Has a mass activity and TOF value of 20.63A/g and 0.005s, respectively-1. FIG. 8 shows Co (OH)2Impedance versus CoP. From the figure, Co (OH) can be seen2Almost completely map the impedance of the CoP to the package. Explanation of Co (OH)2Is greater than the impedance of CoP. So Co (OH)2After the nanosheet is loaded with P, the performance of electrocatalytic oxidation water is greatly improved.
The invention is described above with reference to the accompanying drawings. It is to be understood that the specific implementations of the invention are not limited in this respect. Various insubstantial improvements are made by adopting the method conception and the technical scheme of the invention; the present invention is not limited to the above embodiments, and can be modified in various ways.
Claims (7)
1. A preparation method of a loose structure CoP two-dimensional nanosheet is characterized in that the preparation method comprises the steps of placing a cobalt hydroxide nanosheet serving as a precursor at one end of a porcelain boat, placing sodium metaphosphate at the other end of the porcelain boat, then placing the porcelain boat in a heating furnace protected by inert gas for heating reaction, wherein one end filled with the sodium metaphosphate faces to an air outlet of the heating furnace, then washing, centrifugally collecting and drying products in sequence to obtain the loose structure CoP two-dimensional nanosheet, adding ammonia water into a mixed solution of cobalt acetate and aluminum chloride for stirring reaction, and then subjecting obtained precipitates to high-temperature reaction, centrifugal separation, washing and drying in sequence to obtain a Co (OH)2A two-dimensional nanoplate precursor; the reaction temperature of the high-temperature reaction is 110-130 ℃, the molar ratio of the cobalt acetate to the aluminum chloride solution is 1-4:1, and the volume ratio of the solvent water to the ammonia water in the mixed solution of the cobalt acetate and the aluminum chloride is 5-15: 1; the length of the cobalt hydroxide two-dimensional nano-sheet is 100-150nm, and the thickness is 2-5 nm.
2. The method for preparing loose-structure CoP two-dimensional nanosheets of claim 1, wherein the washing is carried out sequentially with distilled water and ethanol.
3. The preparation method of the loose-structure CoP two-dimensional nanosheet according to claim 1, wherein the drying is carried out by oven drying at a temperature of 60-80 ℃ for 8-24 h.
4. The preparation method of loose-structure CoP two-dimensional nanosheets of claim 1, wherein the mass ratio of sodium metaphosphate to precursor is 5-25: 1.
5. The method for preparing loose-structure CoP two-dimensional nanosheets according to claim 1, wherein the heating reaction is carried out under N2In a protected tube furnace at 2 ℃/minThe temperature rise rate is raised to 300-350 ℃, and the temperature is maintained for 2 h.
6. The preparation method of the loose-structure CoP two-dimensional nanosheet according to claim 1, wherein the washing of the product is carried out by sequentially washing with distilled water and ethanol, and drying is carried out by oven drying at 60-80 ℃ for 8-24 h.
7. The preparation method of loose-structure CoP two-dimensional nanosheets of claim 1, wherein the CoP two-dimensional nanosheets are 100-150nm long and 3-7nm thick.
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