CN113174584A - Porous nitride electrode and preparation method and application thereof - Google Patents

Porous nitride electrode and preparation method and application thereof Download PDF

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CN113174584A
CN113174584A CN202110422271.6A CN202110422271A CN113174584A CN 113174584 A CN113174584 A CN 113174584A CN 202110422271 A CN202110422271 A CN 202110422271A CN 113174584 A CN113174584 A CN 113174584A
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porous
nitride
electrode according
nitride electrode
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黄辉
渠波
陈顺姬
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Abstract

The invention relates to the technical field of electrode materials, in particular to a porous nitride electrode and a preparation method and application thereof. The porous nitride electrode can be used for electrochemical sensors and electrolytic water, and has high surface area, conductivity, catalytic activity and corrosion resistance.

Description

Porous nitride electrode and preparation method and application thereof
Technical Field
The invention relates to the technical field of electrode materials, in particular to a porous nitride electrode and a preparation method and application thereof.
Background
The electrochemical device can be used for detecting the content of trace substances in liquid or gas (electrochemical sensor), and can also be used for producing hydrogen by electrolyzing water in the field of new energy.
In order to improve the performances of the electrochemical device, such as sensitivity, conversion efficiency, etc., the surface area of the electrode needs to be increased, and a common method is to use a nano material, such as nano particles, nano wires or porous thin films, as an electrode material. For the nanoparticle electrode, the nanoparticle needs to be assembled and fixed, and the surface of the nanoparticle cannot be shielded and covered, so that the preparation process of the device electrode is complex, and the stability and reliability are poor; for the nanowire electrode, the nanowire is thin in structure and difficult to arrange and assemble, so that the preparation process of the device electrode is complex; with porous membrane electrodes, it is difficult to form three-dimensional volumetric spaces, and the total surface area is limited.
Gallium nitride (GaN) material belongs to the third generation semiconductor material, and is similar to conventional semiconductor materials such as silicon, GaAs, SnO2Compared with ZnO and the like, the preparation process is mature and reliable, and has excellent stability and conductivity. However, gallium nitride materials do not have chemical catalytic activity and are still deficient in corrosion resistance (particularly in alkaline solutions), which limits their application in the electrochemical field; in addition, the porous gallium nitride film is usually prepared by a chemical etching process at present, and the process is complex.
Disclosure of Invention
The present invention has been made in view of the above-mentioned problems, and an object of the present invention is to provide a porous nitride electrode having high reliability, a large specific surface area, and high catalytic activity.
In order to achieve the purpose, the invention adopts the following technical scheme:
the porous nitride electrode comprises a substrate, a three-dimensional porous skeleton structure deposited on the substrate, and a coating layer coating the three-dimensional porous skeleton structure, wherein the three-dimensional porous skeleton structure comprises one of gallium nitride, indium nitride and aluminum nitride or a composite thereof, and the coating layer comprises one of titanium nitride, cobalt nitride and nickel nitride or a composite thereof.
In the above technical solution, the three-dimensional porous skeleton structure includes a porous membrane, a micro-pillar array, a nanowire array and a composite structure thereof.
Preferably, the three-dimensional porous skeletal structure is a porous membrane.
More preferably, the three-dimensional porous skeleton structure is composed of a porous membrane and a nanowire array or nanowire crossbar network on the surface of the porous membrane.
In the above technical solution, the cladding layer is composed of a cladding layer and a porous film, a nano sheet, a nano wire or a nano tube on the surface of the cladding layer.
Preferably, the coating layer is composed of a cladding layer and a nanosheet on the surface of the cladding layer.
In the above technical solution, the substrate is a sapphire substrate or a silicon substrate.
The preparation method of the porous nitride electrode comprises the following steps:
and growing a layer of three-dimensional porous skeleton structure on the surface of the substrate, and then growing a coating layer on the surface of the three-dimensional porous skeleton to obtain the porous nitride electrode.
In the above technical scheme, the growth method includes any one or a combination of more of metal organic chemical vapor deposition, physical vapor deposition, hydrothermal synthesis, molecular beam epitaxy, thermal evaporation, electron beam evaporation, magnetron sputtering, and electrochemical deposition.
The electrochemical deposition is easy to form a structure (such as a flower-shaped nano sheet) with a large specific surface area, and the sensitivity of the sensor is improved; magnetron sputtering and thermal evaporation are easy to form a thin film structure.
The porous nitride electrode is applied to electrochemical sensors and electrolytic water.
The invention has the beneficial effects that:
(1) the porous nitride electrode contains gallium nitride, indium nitride, aluminum nitride and other materials, belongs to the third-generation semiconductor material, has a mature industrialized growth preparation process, is easy to control the crystal quality (such as doping and nitrogen vacancy introduction) and the form (such as thin film preparation, micron column preparation and nanowire preparation), is easy to prepare a three-dimensional porous skeleton structure, and has the advantages of simple preparation process, stable structure and no need of an adhesive; the materials such as titanium nitride, cobalt nitride, nickel nitride and the like have excellent conductivity, catalytic activity and corrosion resistance, and can be prevented from being corroded and improved in conductivity and stability by coating the surfaces of the three-dimensional porous skeleton structures, so that the sensitivity and stability of the electrode device are improved. The porous nitride electrode provided by the invention overcomes the defects that the conductivity and the corrosion resistance of a three-dimensional porous skeleton structure are poor, and a coating layer is easy to agglomerate.
(2) When the object to be detected is subjected to reduction (or oxidation) reaction on the surface of the nitride electrode, the porous nitride electrode can generate signal current, so that the porous nitride electrode can be used as an electrochemical sensor; when voltage and current are applied to the nitride electrode, hydrogen ions or hydroxyl ions in water undergo reduction or oxidation reaction on the surface of the electrode, so that the water is decomposed into hydrogen and oxygen, and the hydrogen and hydroxyl ions can be used for hydrogen production by water electrolysis.
Drawings
Fig. 1 is a schematic structural view of a porous nitride electrode of example 1.
Fig. 2 is a schematic structural view of a porous nitride electrode of example 2.
Fig. 3 is an electron micrograph of the flower-like nanosheets of example 1.
Fig. 4 is an electron micrograph of the flower-like nanosheets of example 2.
Reference numerals: the nano-film comprises a substrate 1, a porous film 2, flower-shaped nano-sheets 3, nano-wires 5 and a cladding 6.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A method for preparing a porous nitride electrode, comprising the steps of:
growing a layer of gallium nitride porous membrane 2 on the surface of a sapphire substrate 1 at 600-800 ℃ by using a Metal Organic Chemical Vapor Deposition (MOCVD) technology, wherein the gallium nitride porous membrane 2 is provided with dense small holes and abundant nitrogen vacancies;
step two, performing magnetron sputtering on a layer of cobalt-nickel alloy on the surface of the gallium nitride porous membrane 2, and then annealing at 800 ℃ in an ammonia atmosphere to obtain a cobalt-nickel nitride cladding 6;
and step three, placing the substance obtained in the step two in an aqueous solution containing cobalt ions and nickel ions, applying voltage on the surface of the cladding 6 by using an electrochemical deposition method to deposit the cobalt ions and the nickel ions in the aqueous solution on the surface of the cobalt nickel nitride cladding 6 to form cobalt nickel hydroxide, and then placing the cobalt nickel hydroxide in an ammonia atmosphere to anneal at 400-700 ℃ to obtain the cobalt nickel nitride composite flower-shaped nanosheet 3.
The porous nitride electrode of the present embodiment can be used as an electrochemical sensor electrode material.
In this embodiment, the growth temperature of the cobalt nickel nitride composite flower-like nanosheets 3 is preferably 500 ℃.
In this embodiment, the growth temperature of the gallium nitride porous film 2 is preferably 720 ℃; nitrogen vacancies are easily introduced at the growth temperature of 600-800 ℃, so that the catalytic activity and the conductivity of the nitride are improved, and the electrode performance is favorably improved; both ranges fail to yield porous films when the growth temperature is high (e.g., >800 ℃) to form smooth, flat films and when the growth temperature is low (e.g., <600 ℃) to form granular films.
In this embodiment, Co is easily formed when the ammoniation temperature is lower than 500 deg.C3N and Co3N-Ni3Three-dimensional petal-like nanostructures of N (i.e., petal-like nanoplates 3 shown in fig. 3); when the ammoniation temperature is higher than 500 ℃, Co is easily formed5.47N and Co5.47N-NixFlower-like nanosheets 3 of N. The flower-shaped nanosheets 3 of the cobalt-nickel nitride composite have high surface area, conductivity and abundant active sites, and can improve sensitivity and conversion efficiency.
The flower-shaped nanosheets 3 are provided with nanopores, gaps are formed between adjacent flower-shaped nanosheets 3, and the three-dimensional petal-shaped structure is beneficial for a sample (ions or molecules) to be detected to enter and exit the nanopores, so that the response speed of the sensor is high, and a large surface area, namely high sensitivity, can be obtained. The three-dimensional petal-shaped structure is formed by deposition growth, an etching process or a binder is not needed, the structure is firm and stable, and the stability of the sensor is good.
Because the cobalt nickel nitride cladding layer 6 and the flower-shaped nanosheets 3 have good corrosion resistance (namely good chemical stability), the cobalt nickel nitride cladding layer and the flower-shaped nanosheets together clad the gallium nitride porous film 2, so that the gallium nitride porous film 2 is prevented from being corroded by a solution, the stability of the electrode is improved, and the service life of the electrode is prolonged.
Example 2
A method for preparing a porous nitride electrode, comprising the steps of:
growing a layer of aluminum gallium nitrogen porous membrane 2 on the surface of a silicon substrate 1 by using a Chemical Vapor Deposition (CVD) technology at the temperature of 600-900 ℃, wherein the aluminum gallium nitrogen porous membrane 2 is provided with dense small holes and abundant nitrogen vacancies;
growing gallium nitride nanowires 5 on the surface of the aluminum gallium nitrogen porous membrane 2 at 600-800 ℃ by using an MOCVD (metal organic chemical vapor deposition) technology, wherein the gallium nitride nanowires 5 are mutually crossed and interconnected to form a stable three-dimensional porous framework;
thirdly, growing a titanium nitride cladding 6 on the surface of the gallium nitride nanowire 5 by using a CVD (chemical vapor deposition) technology;
step four, putting the substance obtained in the step three in an aqueous solution containing nickel ions, applying voltage on the surface of the cladding 6 by using an electrochemical deposition method to deposit the nickel ions in the aqueous solution on the surface of the titanium nitride cladding 6 to form nickel hydroxide, and then putting the nickel hydroxide in an ammonia atmosphere for annealing at 500 ℃ to obtain the nickel nitride flower-shaped nanosheets 3 (which are mutually crosslinked to form a three-dimensional flower-shaped nanostructure) with high surface area and catalytic activity.
In this embodiment, the growth temperature of the aluminum gallium nitride porous film 2 is preferably 820 ℃, and the growth temperature of the gallium nitride nanowire 5 is preferably 720 ℃.
The nickel nitride flower-shaped nanosheets 3 grow on the three-dimensional framework of the gallium nitride nanowire 5 and the titanium nitride cladding layer 6, so that the nickel nitride flower-shaped nanosheets 3 can be prevented from agglomerating (the flower-shaped nanosheets 3 are dispersed in the three-dimensional framework), and the total surface area can be increased; moreover, the titanium nitride cladding layer 6 and the nickel nitride flower-shaped nanosheets 3 have good corrosion resistance and electrical conductivity, and the gallium nitride nanowires 5 are jointly coated by the titanium nitride cladding layer and the nickel nitride flower-shaped nanosheets, so that the gallium nitride nanowires 5 are prevented from being corroded by the solution, and the service life of the electrode is prolonged. The porous nitride electrode can be used as an electrode material for electrolyzing water.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. A porous nitride electrode, characterized in that: the three-dimensional porous structure comprises a substrate, a three-dimensional porous skeleton structure deposited on the substrate and a coating layer coating the three-dimensional porous skeleton structure, wherein the three-dimensional porous skeleton structure comprises one of gallium nitride, indium nitride and aluminum nitride or a compound thereof, and the coating layer comprises one of titanium nitride, cobalt nitride and nickel nitride or a compound thereof.
2. A porous nitride electrode according to claim 1, wherein: the three-dimensional porous skeleton structure comprises a porous membrane, a micro-column array, a nanowire array and a composite structure of the porous membrane, the micro-column array and the nanowire array.
3. A porous nitride electrode according to claim 2, wherein: the three-dimensional porous skeleton structure is a porous membrane.
4. A porous nitride electrode according to claim 2, wherein: the three-dimensional porous skeleton structure is composed of a porous membrane and a nanowire array or nanowire crossing network on the surface of the porous membrane.
5. A porous nitride electrode according to claim 1, wherein: the coating layer is composed of a coating layer and a porous film, a nano sheet, a nano wire or a nano tube on the surface of the coating layer.
6. The porous nitride electrode according to claim 5, wherein: the coating layer is composed of a cladding layer and a nano sheet on the surface of the cladding layer.
7. A porous nitride electrode according to claim 1, wherein: the substrate is a sapphire substrate or a silicon substrate.
8. The method for producing a porous nitride electrode according to any one of claims 1 to 7, wherein: and growing a layer of three-dimensional porous skeleton structure on the surface of the substrate, and then growing a coating layer on the surface of the three-dimensional porous skeleton to obtain the porous nitride electrode.
9. The method for preparing a porous nitride electrode according to claim 8, wherein: the growth method comprises any one or more of metal organic chemical vapor deposition, physical vapor deposition, hydrothermal synthesis, molecular beam epitaxy, thermal evaporation, electron beam evaporation, magnetron sputtering and electrochemical deposition.
10. Use of a porous nitride electrode according to any one of claims 1-7 in electrochemical sensors and in electrolysis of water.
CN202110422271.6A 2021-01-16 2021-04-20 Porous nitride electrode and preparation method and application thereof Pending CN113174584A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5750438A (en) * 1996-06-04 1998-05-12 United Microelectronics Corporation Method for fabricating a local interconnection structure
US20060067871A1 (en) * 2004-05-26 2006-03-30 Massachusetts Institute Of Technology Methods and devices for growth and/or assembly of nanostructures
US8377728B1 (en) * 2011-10-07 2013-02-19 Tsinghua University Method for making light emitting diode
CN105845714A (en) * 2016-02-27 2016-08-10 黄辉 Nanowire device based on bridging growth and manufacturing method thereof
CN106770543A (en) * 2016-08-27 2017-05-31 黄辉 A kind of electrochemical sensor based on nano wire microelectrode
CN107243356A (en) * 2017-04-06 2017-10-13 山东大学 A kind of elctro-catalyst and its application with nickel cobalt nitride three-dimensional structure
CN109637822A (en) * 2018-12-19 2019-04-16 大连理工大学 A kind of TiN electrode of high-specific surface area, preparation method and applications
CN110412082A (en) * 2019-06-20 2019-11-05 黄辉 A kind of semiconductor porous crystalline thin films sensor and preparation method
CN111261428A (en) * 2020-02-27 2020-06-09 三峡大学 Method for enhancing performance of cobalt nickel sulfide supercapacitor by ammonia plasma

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5750438A (en) * 1996-06-04 1998-05-12 United Microelectronics Corporation Method for fabricating a local interconnection structure
US20060067871A1 (en) * 2004-05-26 2006-03-30 Massachusetts Institute Of Technology Methods and devices for growth and/or assembly of nanostructures
US8377728B1 (en) * 2011-10-07 2013-02-19 Tsinghua University Method for making light emitting diode
CN105845714A (en) * 2016-02-27 2016-08-10 黄辉 Nanowire device based on bridging growth and manufacturing method thereof
CN106770543A (en) * 2016-08-27 2017-05-31 黄辉 A kind of electrochemical sensor based on nano wire microelectrode
CN107243356A (en) * 2017-04-06 2017-10-13 山东大学 A kind of elctro-catalyst and its application with nickel cobalt nitride three-dimensional structure
CN109637822A (en) * 2018-12-19 2019-04-16 大连理工大学 A kind of TiN electrode of high-specific surface area, preparation method and applications
CN110412082A (en) * 2019-06-20 2019-11-05 黄辉 A kind of semiconductor porous crystalline thin films sensor and preparation method
CN111261428A (en) * 2020-02-27 2020-06-09 三峡大学 Method for enhancing performance of cobalt nickel sulfide supercapacitor by ammonia plasma

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