CN115094455B - CoTe 2 CoP@Ti composite material and preparation method thereof - Google Patents
CoTe 2 CoP@Ti composite material and preparation method thereof Download PDFInfo
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Abstract
Embodiments of the present application provide a CoTe 2 The preparation method of the CoP@Ti composite material comprises the steps of preparing a Co source mixed solution A, and preprocessing a titanium mesh; mixing the Co source mixed solution A with the pretreated titanium mesh to perform hydrothermal reaction to obtain an intermediate product B; then, carrying out one-step phosphating and telluride reaction on the intermediate product B and sodium hypophosphite and tellurium powder to obtain a target product CoTe2/CoP@Ti composite material; coTe grown on Ti net is obtained by hydrothermal synthesis and one-step simple gas phase reaction method 2 CoTe prepared from CoP@Ti composite electrode material 2 the/CoP@Ti composite material is of a one-dimensional nanowire structure; coTe 2 The CoP grows on the Ti net uniformly and vertically and shows nano array distribution; coTe 2 The CoP@Ti composite material has an open space, is more favorable for the permeation and bubble release of electrolyte, and has the characteristics of hydrophilic and hydrophobic, so that more active sites are exposed and the mass transfer process is enhanced, thereby improving the efficiency of the electrocatalyst.
Description
Technical Field
The application relates to the technical field of nano materials and new energy materials, in particular to CoTe 2 A/CoP@Ti composite material and a preparation method thereof.
Background
The hydrogen energy has wide source, clean (zero carbon emission) and high energy density (142 MJkg) -1 ) And the like, is considered as an ultimate energy carrier of human beings, and is also an important way for upgrading energy and environmental protection. The main mode of hydrogen sources is fossil fuel gasification reforming, but the conditions of high temperature and the like are needed in the production process, so that serious environmental pollution, noise pollution and the like are brought, and the electrocatalytic water decomposition hydrogen production method has the characteristics of simple process, no pollution in the production process, high purity of the produced hydrogen and the like, meets the requirement of sustainable green development, and is also an important measure for realizing a double-carbon strategy. Noble metal catalysts are still considered to be the most active water electrolysis catalysts at present, but the rapid development of water electrolysis technology is hampered by the high price. Therefore, the development of a new material with high activity, high stability and low cost has important significance for improving the hydrogen production technology by water electrolysis.
The single metal phosphide and telluride catalysts have poor activity, and the hetero-junction interface CoTe can be constructed due to the existence of poor electronegativity of anions Te and P 2 According to the CoP, the interface is different in atomic coordination mode, so that the electronic structure of an active site is rearranged, the catalytic activity is improved, but the difficulty of realizing accurate compounding of a two-phase material is high, although the preparation of Ni by hydrothermal telluride and then phosphating is reported at present 2 P/NiTe 2 The catalyst, however, is cumbersome.
The present application has been made in view of this.
Disclosure of Invention
To solve one of the above technical drawbacks, an embodiment of the present application provides a CoTe 2 A/CoP@Ti composite material and a preparation method thereof. CoTe grown on Ti net is obtained by hydrothermal synthesis and one-step simple gas phase reaction method 2 CoTe prepared from CoP@Ti composite electrode material 2 the/CoP@Ti composite material is of a one-dimensional nanowire structure; coTe 2 The CoP grows on the Ti net uniformly and vertically and shows nano array distribution; coTe 2 The open space exists in the/CoP@Ti composite material, which is more beneficial to electricityPermeation of the electrolyte and release of the gas bubbles, exhibit hydrophilic character, thereby exposing more active sites and enhancing the mass transfer process, thereby improving the efficiency of the electrocatalyst.
In order to achieve the above purpose, the present application adopts the following technical scheme:
CoTe 2 The preparation method of the CoP@Ti composite material comprises the steps of preparing a Co source mixed solution A, and preprocessing a titanium mesh; mixing the Co source mixed solution A with the pretreated titanium mesh to perform hydrothermal reaction to obtain an intermediate product B; then the intermediate product B and sodium hypophosphite and tellurium powder are subjected to one-step phosphating and telluride reaction to obtain the target product CoTe 2 CoP@Ti composite material.
Preferably, a CoTe 2 The preparation method of the/CoP@Ti composite material comprises the following specific steps:
(1) Carrying out ultrasonic pretreatment on the titanium mesh;
(2) Co (NO) 3 ) 2 ·6H 2 O、CO(NH 2 ) 2 NH and NH 4 F, dissolving in an aqueous solution, and stirring until the solution is completely dissolved to obtain a Co source mixed solution A; the addition of ammonium fluoride provides the effect of controlling the shape of the nanowire;
(3) Adding the Co source mixed solution A prepared in the step (2) into a reaction kettle, adding the titanium mesh treated in the step (1), sealing, and performing hydrothermal reaction; cooling the hydrothermal reaction product to room temperature, and then drying to obtain an intermediate product B;
(4) Respectively placing sodium hypophosphite, tellurium powder and the intermediate product B prepared in the step (3) in corresponding containers, and carrying out one-step phosphorization and tellurium reaction to obtain a target product CoTe 2 CoP@Ti composite material.
Preferably, the ultrasonic pretreatment of the titanium mesh specifically comprises the following steps: cutting the titanium mesh into a preset size, soaking in concentrated hydrochloric acid, performing ultrasonic treatment to remove an oxide layer on the surface, and then respectively performing ultrasonic cleaning with deionized water and ethanol.
Preferably, co (NO 3 ) 2 ·6H 2 O、CO(NH 2 ) 2 NH and NH 4 The molar ratio of F is 1 (2.5-4) to 2-4.
Preferably, the mass ratio of the sodium hypophosphite to the tellurium powder to the intermediate product B prepared in the step (3) is 20:10 (1-5).
Preferably, the step (4) specifically includes: respectively and sequentially placing sodium hypophosphite, tellurium powder and the intermediate product B prepared in the step (3) in a porcelain boat, and calcining in a tube furnace to perform one-step phosphorization and tellurium reaction to obtain a target product CoTe 2 CoP@Ti composite material. Decomposing sodium hypophosphite and tellurium powder into PH at high temperature under the condition of hydrogen-argon mixed gas 3 And TeH 3 Respectively synthesizing with the intermediate products to generate target products.
Preferably, the reaction conditions in the tube furnace are: 10% H 2 Under the Ar atmosphere, the air flow is 100sccm, the heating rate is 1-3 ℃/min, and the temperature is kept for 1-3 h at 300-400 ℃.
The application also provides a CoTe 2 The CoP@Ti composite material is prepared by adopting the preparation method; the CoTe is 2 the/CoP@Ti composite material is of a one-dimensional nanowire structure; coTe 2 The CoP uniformly and vertically grows on the Ti net and presents nano array distribution; there is an open space; the CoTe is 2 the/CoP@Ti has a hydrophilic characteristic.
The application has the following beneficial effects:
1. the composite electrode material prepared by the application is in a nano array shape, the diameter is about 100-200nm, meanwhile, because Te and P anions in two phases of the composite material are different in electronegativity, electron transfer at the interface can be realized by constructing a heterojunction interface, and because the coordination mode at the interface is different from that of respective bulk phase materials, the electronic structure at the interface is definitely different from the bulk phase, and the existence of the heterojunction interface is also an important means for improving the activity of a catalyst, the interface effect at the interface of the composite material causes the change of the coordination mode at the interface, and the redistribution of the electronic structure at the interface causes the cooperative improvement of the catalytic activity and the stability of the electrode material.
2. The application firstly utilizes hydrothermal synthesis to prepare intermediate product B, namely Co generates intermediate product Co (OH) F under alkaline hydrothermal condition, and the intermediate product B is obtained by a one-step simple gas phase reaction method, namely one-step phosphating and tellurizing reactionCoTe grown on Ti net 2 CoTe prepared from CoP@Ti composite electrode material 2 the/CoP@Ti composite material is of a one-dimensional nanowire structure; coTe 2 CoP uniformly grows vertically on Ti net and CoTe 2 The CoP presents nano array distribution in the Ti net; because of the vertical growth, open space exists, which is more favorable for the permeation of electrolyte and the release of bubbles, and shows hydrophilic characteristics, thereby exposing more active sites and enhancing the mass transfer process, thereby improving the efficiency of the electrocatalyst.
Description of the drawings:
the accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute a limitation on the application.
FIG. 1 shows CoTe prepared in accordance with an embodiment of the present application 2 A nanowire array scan of CoP on Ti mesh;
FIG. 2 shows CoTe prepared in accordance with an embodiment of the present application 2 Contact angle test pattern of/CoP;
FIG. 3 is an XPS diagram of Co 2p in three materials prepared in the examples of the present application;
FIG. 4 is a graph showing electrochemical hydrogen evolution performance of different materials prepared according to an embodiment of the present application.
Detailed Description
In order to make the technical solutions and advantages of the embodiments of the present application more apparent, the following detailed description of exemplary embodiments of the present application is provided in conjunction with the accompanying drawings, and it is apparent that the described embodiments are only some embodiments of the present application and not exhaustive of all embodiments. It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other.
Example 1
(1) Firstly, cutting a titanium net into 4 x 2cm pieces 2 Soaking in concentrated hydrochloric acid for 10min for ultrasonic treatment to remove the oxide layer on the surface of the titanium mesh, and then respectively carrying out ultrasonic cleaning for 3 times by using deionized water and ethanol;
(2)1mmol Co(NO 3 ) 2 ·6H 2 O，4mmol CO(NH 2 ) 2 and 1.67mmol NH 4 F is dissolved in 40mL of water solution, and stirring is carried out until the solution is completely dissolved to obtain Co source mixed solution A;
(3) Adding the Co source mixed solution A prepared in the step (2) into a reaction kettle, adding the titanium mesh treated in the step (1), sealing, and carrying out hydrothermal reaction at a heating rate of 3 ℃/min and a temperature of 120 ℃ for 6 hours; cooling the hydrothermal reaction product to room temperature, cleaning a sample growing on a titanium net with deionized water for three times, and then carrying out vacuum drying at 60 ℃ for 12 hours; then drying to obtain an intermediate product B;
(4) 400mg sodium hypophosphite, 30mg tellurium powder and vacuum dried sample (1.5 x 2cm 2 ) Respectively put in a porcelain boat in turn, then 10% H 2 And (3) carrying out gas phase reaction in a tube furnace at a gas flow rate of 100sccm under Ar atmosphere, and preserving heat at a temperature rising rate of 2 ℃/min and a temperature of 350 ℃ for two hours.
Example two
(1) Firstly, cutting a titanium net into 4 x 2cm pieces 2 Soaking in concentrated hydrochloric acid for 10min for ultrasonic treatment to remove the oxide layer on the surface of the titanium mesh, and then respectively carrying out ultrasonic cleaning for 3 times by using deionized water and ethanol;
(2)1mmol Co(NO 3 ) 2 ·6H 2 O，2.5mmol CO(NH 2 ) 2 and 1.67mmol NH 4 F is dissolved in 40mL of water solution, and stirring is carried out until the solution is completely dissolved to obtain Co source mixed solution A;
(3) Adding the Co source mixed solution A prepared in the step (2) into a reaction kettle, adding the titanium mesh treated in the step (1), sealing, and carrying out hydrothermal reaction at a heating rate of 3 ℃/min and a temperature of 120 ℃ for 6 hours; cooling the hydrothermal reaction product to room temperature, cleaning a sample growing on a titanium net with deionized water for three times, and then carrying out vacuum drying at 60 ℃ for 12 hours; then drying to obtain an intermediate product B;
(4) 400mg sodium hypophosphite, 30mg tellurium powder and vacuum dried sample (1.5 x 2cm 2 ) Respectively put in a porcelain boat in turn, then 10% H 2 In Ar atmosphere, the gas flow is 100sccm, the gas phase reaction is carried out in a tube furnace, the heating rate is 2 ℃/min, and the temperature is kept at 350 DEG CTwo hours.
Example III
(1) Firstly, cutting a titanium net into 4 x 2cm pieces 2 Soaking in concentrated hydrochloric acid for 10min for ultrasonic treatment to remove the oxide layer on the surface of the titanium mesh, and then respectively carrying out ultrasonic cleaning for 3 times by using deionized water and ethanol;
(2)1mmol Co(NO 3 ) 2 ·6H 2 O，4mmol CO(NH 2 ) 2 and 4mmol NH 4 F is dissolved in 40mL of water solution, and stirring is carried out until the solution is completely dissolved to obtain Co source mixed solution A;
(3) Adding the Co source mixed solution A prepared in the step (2) into a reaction kettle, adding the titanium mesh treated in the step (1), sealing, and carrying out hydrothermal reaction at a heating rate of 3 ℃/min and a temperature of 120 ℃ for 6 hours; cooling the hydrothermal reaction product to room temperature, cleaning a sample growing on a titanium net with deionized water for three times, and then carrying out vacuum drying at 60 ℃ for 12 hours; then drying to obtain an intermediate product B;
(4) 400mg sodium hypophosphite, 30mg tellurium powder and vacuum dried sample (1.5 x 2cm 2 ) Respectively put in a porcelain boat in turn, then 10% H 2 And (3) carrying out gas phase reaction in a tube furnace at a gas flow rate of 100sccm under Ar atmosphere, and preserving heat at a temperature rising rate of 2 ℃/min and a temperature of 350 ℃ for two hours.
As shown in FIG. 1, coTe 2 The map of the nanowire array on the Ti net by CoP shows that the appearance is one-dimensional nanowire (200 nm) obviously from the map, and the nanowire vertically grows on the Ti net and is in the shape of the nanowire array, so that the nanowire array has high surface area.
As shown in FIG. 2, it can be seen that the target product CoTe of the present application 2 The CoP has good super-wettability; as the catalytic reaction is carried out in the aqueous solution, the characteristic of super wettability is favorable for fully contacting the catalyst material with the electrolyte, the mass transfer and charge capacity of the catalyst and the electrolyte are improved, and the catalytic activity of the material is improved.
From the X-ray photoelectron spectrum in fig. 3, it is shown that the binding energy of the target material is significantly cheaper, and compared with the single-phase material, co 2p3/2 is located in the middle of the two-phase material, resulting in electron transfer and improved electronic structure.
FIG. 4 is a graph showing electrochemical hydrogen evolution performance of different materials, from which it can be seen that the target product CoTe 2 The activity of/CoP is better.
Based on the above, embodiments of the present application one-dimensional CoTe 2 The CoP@Ti nano electrode material has high surface area, is beneficial to surface reaction, and meanwhile, the one-dimensional nano structure can provide continuous electron and ion transmission channels, so that mass transfer and charge transfer processes in electrochemical reaction can be accelerated. The array structure formed by the one-dimensional nanowires has an open space, is more favorable for the permeation and bubble release of electrolyte, and shows the characteristics of hydrophilic and hydrophobic, so that more active sites are exposed and the mass transfer process is enhanced, thereby improving the efficiency of the electrocatalyst.
While preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the application.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present application without departing from the spirit or scope of the application. Thus, it is intended that the present application also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (5)
1. CoTe 2 The preparation method of the CoP@Ti composite material is characterized by preparing a Co source mixed solution A and preprocessing a titanium mesh; mixing the Co source mixed solution A with the pretreated titanium mesh to perform hydrothermal reaction to obtain an intermediate product B; then the intermediate product B and sodium hypophosphite and tellurium powder are subjected to one-step phosphating and telluride reaction to obtain the target product CoTe 2 a/CoP@Ti composite material;
the method comprises the following specific steps:
(1) Carrying out ultrasonic pretreatment on the titanium mesh;
(2) Co (NO) 3 ) 2 ·6H 2 O、CO(NH 2 ) 2 NH and NH 4 F, dissolving in an aqueous solution, and stirring until the solution is completely dissolved to obtain a Co source mixed solution A;
(3) Adding the Co source mixed solution A prepared in the step (2) into a reaction kettle, adding the titanium mesh treated in the step (1), sealing, and performing hydrothermal reaction; cooling the hydrothermal reaction product to room temperature, and then drying to obtain an intermediate product B;
(4) Respectively placing sodium hypophosphite, tellurium powder and the intermediate product B prepared in the step (3) in corresponding containers, and carrying out one-step phosphorization and tellurium reaction to obtain a target product CoTe 2 a/CoP@Ti composite material;
the step (4) is specifically as follows: respectively and sequentially placing sodium hypophosphite, tellurium powder and the intermediate product B prepared in the step (3) in a porcelain boat, and calcining in a tube furnace to perform one-step phosphorization and tellurium reaction to obtain a target product CoTe 2 a/CoP@Ti composite material;
the reaction conditions in the tube furnace are: 10% H 2 Under the Ar atmosphere, the air flow is 100sccm, the heating rate is 1-3 ℃/min, and the temperature is kept for 1-3 h at 300-400 ℃.
2. The CoTe of claim 1 2 The preparation method of the/CoP@Ti composite material is characterized by comprising the following steps of: cutting the titanium mesh into a preset size, soaking in concentrated hydrochloric acid, performing ultrasonic treatment to remove an oxide layer on the surface, and then respectively performing ultrasonic cleaning with deionized water and ethanol.
3. The CoTe of claim 1 2 A process for preparing the CoP@Ti composite material characterized by that Co (NO 3 ) 2 ·6H 2 O、CO(NH 2 ) 2 NH and NH 4 The molar ratio of F is 1 (2.5-4) to 1.5-4.
4. The CoTe of claim 1 2 The preparation method of the CoP@Ti composite material is characterized by comprising the following steps of20:10 (1-5).
5. CoTe 2 A cop@ti composite material prepared by the preparation method according to any one of claims 1 to 4; the CoTe is 2 the/CoP@Ti composite material is of a one-dimensional nanowire structure; coTe 2 The CoP uniformly and vertically grows on the Ti net and presents nano array distribution; there is an open space; the CoTe is 2 the/CoP@Ti has a hydrophilic characteristic.
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