CN111474213B - Three-layer cylindrical composite graphene-based hydrogen sensor and preparation method thereof - Google Patents
Three-layer cylindrical composite graphene-based hydrogen sensor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a three-layer cylindrical composite graphene-based hydrogen sensor which comprises an upper electrode, a lower electrode and a middle composite structure positioned between the upper electrode and the lower electrode2The middle layer is a foam nickel substrate layer, the outer layer is a graphene net-shaped structure layer, the upper end of the three-layer composite cylindrical structure is connected with the upper electrode in a sealing mode, and the lower end of the three-layer composite cylindrical structure is connected with the lower electrode in a sealing mode. In the three-layer composite cylindrical structure, the graphene net-shaped structure layer is used as an outgoing part, so that the contact area between the sensor and the gas to be detected can be remarkably increased, the response sensitivity of the sensor relative to hydrogen is improved, the drying of some impurity gases to the sensor can be eliminated, and the accuracy of the sensor to hydrogen detection is improved.
Description
Technical Field
The invention belongs to the field of sensors, and particularly relates to a three-layer cylindrical composite graphene-based hydrogen sensor and a preparation method thereof.
Background
Hydrogen is an important reducing gas and is widely applied to various fields of chemical industry, petrifaction, medical treatment and the like. Meanwhile, hydrogen is an important clean energy source, and the combustion of hydrogen can release high energy, so that the hydrogen can be widely applied to various fields such as fuel cells, energy sources and the like. However, hydrogen has a certain safety hazard in practical application, and when the hydrogen content in the air in a local range is more than 4%, explosion is very easy to occur. Moreover, hydrogen molecules are very small, so that the hydrogen can easily leak in the actual production and transportation processes. In addition, hydrogen molecules are colorless and tasteless, are not easy to detect, and have higher potential safety hazard than other gases. It is of great significance to develop a hydrogen sensor that can effectively monitor the concentration of hydrogen.
The hydrogen sensor is used for detecting the concentration of hydrogen in the air, so that the leakage of the hydrogen can be effectively monitored. As for the material, the conventional hydrogen sensor mainly includes a semiconductor type metal oxide sensor and a metal thin film type sensor. The semiconductor type metal oxide sensor has harsh working conditions and high energy consumption; metal film type sensors have limited sensitivity to hydrogen and are relatively costly.
Graphene, as a novel material, has a unique two-dimensional honeycomb crystal structure, and is endowed with excellent physicochemical properties, such as a large specific surface area, good conductivity, chemical stability and the like, and the theoretical thickness of the graphene is only the diameter of one carbon atom and is about 0.14 nm. These excellent properties make graphene a pet in the fabrication of various types of sensors. However, the existing graphene-based sensor generally has the defects of insufficient sensitivity, insufficient corresponding effectiveness or detection accuracy of the sensor and the like.
Based on the three-layer cylindrical composite graphene-based hydrogen sensor, the three-layer cylindrical composite graphene-based hydrogen sensor is high in sensitivity, high in corresponding speed and high in detection precision.
Disclosure of Invention
Based on the defects of the hydrogen sensor in the background art, the invention provides a three-layer cylindrical composite graphene-based hydrogen sensor and a preparation method thereof.
The three-layer cylindrical composite graphene-based hydrogen sensor comprises an upper electrode, a lower electrode and a middle composite structure positioned between the upper electrode and the lower electrode, and is characterized in that the middle composite structure is a three-layer composite cylindrical structure, and the inner layer of the three-layer composite cylindrical structure is SnO2The middle layer is a foam nickel substrate layer, the outer layer is a graphene net-shaped structure layer, the upper end of the three-layer composite cylindrical structure is connected with the upper electrode in a sealing mode, and the lower end of the three-layer composite cylindrical structure is connected with the lower electrode in a sealing mode.
Further, a plurality of intermediate composite structures arranged in parallel may be included between the upper electrode and the lower electrode, and connected in parallel with the upper electrode and the lower electrode, which may further improve the corresponding sensitivity of the hydrogen sensor to hydrogen.
Further, the plurality of intermediate composite structures arranged in parallel are arranged in a single row, in a cross-shaped array, in a matrix in a shape of a Chinese character 'mi', or in a matrix in a shape of a square.
Further, the diameter of the three-layer composite cylindrical structure is 0.5mm-5mm, and the height of the three-layer composite cylindrical structure is 3mm-15 mm.
Further, in the three-layer composite cylindrical structure, SnO2The thickness of the layer is 50nm-1 um; the thickness of the graphene net-shaped structure layer is 50nm-500 nm; the thickness of the foam nickel base layer is 20-100 um.
The preparation method of the three-layer cylindrical composite graphene-based hydrogen sensor comprises the following steps:
(1) pretreatment of a planar flexible foamed nickel substrate: taking planar flexible foamed nickel as a substrate, cleaning and pretreating the planar flexible foamed nickel, sequentially adopting ethanol, acetone and deionized water for ultrasonic cleaning, and then drying for later use;
(2) magnetron sputtering deposition of SnO2Layer (b): transferring the cleaned planar flexible foamed nickel serving as a matrix into a magnetron sputtering device, and using SnO2The ceramic target is a sputtering target, and SnO is obtained by magnetron sputtering2A layer; the specific process parameters are as follows: background vacuum degree of 1X 10- 4Pa, 10% O by volume2The mixed gas of +90% Ar is sputtering gas, the sputtering pressure is 0.5-3Pa, the sputtering power is 200-400W, the sputtering time is 10-100min, and SnO is sputtered and deposited on one side of the planar flexible foamed nickel substrate2A layer;
(3) chemical vapor deposition of a graphene network structure layer: sputter deposited with SnO2Transferring the planar flexible foamed nickel substrate of the layer into a chemical vapor deposition device, and performing chemical vapor deposition on a graphene net-shaped structure layer on the other side of the planar flexible foamed nickel substrate; the specific process parameters are as follows: the flow rate of methane is 20-80sccm, the flow rate of hydrogen is 40-100sccm, the flow rate of Ar is 20-50sccm, the reaction pressure is controlled at 1-5Pa, the deposition temperature is 300-;
(4) bending into a three-layer composite cylindrical structure: will deposit SnO2Winding the planar flexible foam nickel substrate with the layer and the graphene net-shaped structure layer into a cylindrical structure, and bonding the gap with a conductive adhesive to obtain the planar flexible foam nickel substrate with the SnO inner layer2The composite structure comprises a layer, a middle layer and an outer layer, wherein the middle layer is a foam nickel substrate layer, and the outer layer is a three-layer composite cylindrical structure of a graphene net structure layer;
(5) connection of upper and lower electrodes: and (3) hermetically connecting the upper end and the lower end of the three-layer composite cylindrical structure with the upper electrode and the lower electrode respectively.
In the hydrogen sensor, the electrode sensitive to hydrogen has an inner SnO layer2The middle layer is a foam nickel substrate layer, and the outer layer is a graphene net structureThe three-layer composite cylindrical structure of the layers comprises a foam nickel base layer in the middle and SnO in the inner part, wherein the foam nickel base layer is coated by a graphene net structure2The layer is formed into a cylindrical structure, so that the contact area of the sensor and the detected gas can be remarkably increased, and the response sensitivity of the sensor relative to hydrogen is improved.
In the hydrogen sensor of the present invention, a plurality of intermediate composite structures arranged in parallel may be further disposed between the upper electrode and the lower electrode, and connected to the upper electrode and the lower electrode in parallel, so as to further improve the corresponding sensitivity of the hydrogen sensor to hydrogen and enhance the corresponding detection signal strength.
In the hydrogen sensor, the outermost layer is a graphene net structure, the net structure has a certain filtering effect on gas molecules with larger diameters, so that impurity gases can be removed from drying the sensor, and the accuracy of the sensor on hydrogen detection is improved.
Detailed Description
In order to make the technical solution and the advantages of the present invention more clear and obvious, the following detailed description is given with reference to the preferred embodiments of the present invention. It is clear that the following examples are not all the subject of the present invention.
Example 1
The three-layer cylindrical composite graphene-based hydrogen sensor comprises an upper electrode, a lower electrode and a middle composite structure positioned between the upper electrode and the lower electrode, and is characterized in that the middle composite structure is a three-layer composite cylindrical structure, and the inner layer of the three-layer composite cylindrical structure is SnO2The middle layer is a foam nickel substrate layer, the outer layer is a graphene net-shaped structure layer, the upper end of the three-layer composite cylindrical structure is connected with the upper electrode in a sealing mode, and the lower end of the three-layer composite cylindrical structure is connected with the lower electrode in a sealing mode.
The diameter of the three-layer composite cylindrical structure is 3mm, and the height of the three-layer composite cylindrical structure is 9 mm.
In the three-layer composite cylindrical structure, SnO2The thickness of the layer is 180 nm; the thickness of the graphene net-shaped structure layer is 260 nm; the thickness of the foam nickel base layer is 40 um.
The preparation method of the three-layer cylindrical composite graphene-based hydrogen sensor comprises the following steps:
(1) pretreatment of a planar flexible foamed nickel substrate: taking planar flexible foamed nickel as a substrate, cleaning and pretreating the planar flexible foamed nickel, sequentially adopting ethanol, acetone and deionized water for ultrasonic cleaning, and then drying for later use;
(2) magnetron sputtering deposition of SnO2Layer (b): transferring the cleaned planar flexible foamed nickel serving as a matrix into a magnetron sputtering device, and using SnO2The ceramic target is a sputtering target, and SnO is obtained by reactive magnetron sputtering2A layer; the specific process parameters are as follows: background vacuum degree of 1X 10-4Pa, 10% O by volume2The mixed gas of +90% Ar is sputtering gas, the sputtering pressure is 1Pa, the sputtering power is 250W, SnO is sputtered and deposited on one side of the planar flexible foam nickel substrate2A layer;
(3) chemical vapor deposition of a graphene network structure layer: sputter deposited with SnO2Transferring the planar flexible foamed nickel substrate of the layer into a chemical vapor deposition device, and performing chemical vapor deposition on a graphene net-shaped structure layer on the other side of the planar flexible foamed nickel substrate; the specific process parameters are as follows: the flow rate of methane is 40sccm, the flow rate of hydrogen is 40sccm, the flow rate of Ar is 30sccm, the reaction pressure is controlled to be 3Pa, and the deposition temperature is 400 ℃;
(4) bending into a three-layer composite cylindrical structure: will deposit SnO2Winding the planar flexible foam nickel substrate with the layer and the graphene net-shaped structure layer into a cylindrical structure, and bonding the gap with a conductive adhesive to obtain the planar flexible foam nickel substrate with the SnO inner layer2The composite structure comprises a layer, a middle layer and an outer layer, wherein the middle layer is a foam nickel substrate layer, and the outer layer is a three-layer composite cylindrical structure of a graphene net structure layer;
(5) connection of upper and lower electrodes: and (3) hermetically connecting the upper end and the lower end of the three-layer composite cylindrical structure with the upper electrode and the lower electrode respectively.
Example 2
The three-layer cylindrical composite graphene-based hydrogen sensor comprises an upper electrode, a lower electrode and a middle composite structure positioned between the upper electrode and the lower electrode, and is characterized in that the middle composite structure is a three-layer composite cylindrical knotThe inner layer of the three-layer composite cylindrical structure is SnO2The middle layer is a foam nickel substrate layer, the outer layer is a graphene net-shaped structure layer, the upper end of the three-layer composite cylindrical structure is connected with the upper electrode in a sealing mode, and the lower end of the three-layer composite cylindrical structure is connected with the lower electrode in a sealing mode.
Further, a plurality of intermediate composite structures may be included between the upper electrode and the lower electrode, and connected in parallel to the upper electrode and the lower electrode, the plurality of intermediate composite structures being arranged in a matrix in a shape of a Chinese character 'mi'.
The diameter of the three-layer composite cylindrical structure is 4mm, and the height of the three-layer composite cylindrical structure is 15 mm.
In the three-layer composite tubular structure, the SnO2The thickness of the layer is 300 nm; the thickness of the graphene net-shaped structure layer is 400 nm; the thickness of the foam nickel base layer is 80 um.
The preparation method of the three-layer cylindrical composite graphene-based hydrogen sensor comprises the following steps:
(1) pretreatment of a planar flexible foamed nickel substrate: taking planar flexible foamed nickel as a substrate, cleaning and pretreating the planar flexible foamed nickel, sequentially adopting ethanol, acetone and deionized water for ultrasonic cleaning, and then drying for later use;
(2) magnetron sputtering deposition of SnO2Layer (b): transferring the cleaned planar flexible foamed nickel serving as a matrix into a magnetron sputtering device, and using SnO2The ceramic target is a sputtering target, and SnO is obtained by reactive magnetron sputtering2A layer; the specific process parameters are as follows: background vacuum degree of 1X 10-4Pa, 10% O by volume2The mixed gas of +90% Ar is sputtering gas, the sputtering pressure is 2Pa, the sputtering power is 350W, SnO is sputtered and deposited on one side of the planar flexible foam nickel substrate2A layer;
(3) chemical vapor deposition of a graphene network structure layer: sputter deposited with SnO2Transferring the planar flexible foamed nickel substrate of the layer into a chemical vapor deposition device, and performing chemical vapor deposition on a graphene net-shaped structure layer on the other side of the planar flexible foamed nickel substrate; the specific process parameters are as follows: the flow rate of methane was 70sccm, the flow rate of hydrogen was 60sccm, and the flow rate of Ar was 50sccmThe pressure is controlled to be 4Pa, and the deposition temperature is 450 ℃;
(4) bending into a three-layer composite cylindrical structure: will deposit SnO2Winding the planar flexible foam nickel substrate with the layer and the graphene net-shaped structure layer into a cylindrical structure, and bonding the gap with a conductive adhesive to obtain the planar flexible foam nickel substrate with the SnO inner layer2The composite structure comprises a layer, a middle layer and an outer layer, wherein the middle layer is a foam nickel substrate layer, and the outer layer is a three-layer composite cylindrical structure of a graphene net structure layer;
(5) connection of upper and lower electrodes: and hermetically connecting the upper ends and the lower ends of a plurality of three-layer composite cylindrical structures which are arrayed in a shape of a Chinese character 'mi' with the upper electrode and the lower electrode respectively.
Example 3
The three-layer cylindrical composite graphene-based hydrogen sensor comprises an upper electrode, a lower electrode and a middle composite structure positioned between the upper electrode and the lower electrode, and is characterized in that the middle composite structure is a three-layer composite cylindrical structure, the inner layer of the three-layer composite cylindrical structure is a SnO2 layer, the middle layer is a foam nickel base layer, the outer layer is a graphene net-shaped structure layer, the upper end of the three-layer composite cylindrical structure is connected with the upper electrode in a sealing mode, and the lower end of the three-layer composite cylindrical structure is connected with the lower electrode in a sealing mode.
Further, a plurality of intermediate composite structures may be included between the upper electrode and the lower electrode, and connected to the upper electrode and the lower electrode in parallel, the plurality of intermediate composite structures being arranged in a matrix in a square shape.
The diameter of the three-layer composite cylindrical structure is 0.5mm, and the height of the three-layer composite cylindrical structure is 3 mm.
In the three-layer composite tubular structure, the SnO2The thickness of the layer is 50 nm; the thickness of the graphene net-shaped structure layer is 100 nm; the thickness of the foam nickel base layer is 20 um.
The preparation method of the three-layer cylindrical composite graphene-based hydrogen sensor comprises the following steps:
(1) pretreatment of a planar flexible foamed nickel substrate: taking planar flexible foamed nickel as a substrate, cleaning and pretreating the planar flexible foamed nickel, sequentially adopting ethanol, acetone and deionized water for ultrasonic cleaning, and then drying for later use;
(2) magnetron sputtering deposition of SnO2Layer (b): transferring the cleaned planar flexible foamed nickel serving as a matrix into a magnetron sputtering device, and using SnO2The ceramic target is a sputtering target, and SnO is obtained by reactive magnetron sputtering2A layer; the specific process parameters are as follows: background vacuum degree of 1X 10-4Pa, 10% O by volume2The mixed gas of +90% Ar is sputtering gas, the sputtering pressure is 1Pa, the sputtering power is 200W, SnO is sputtered and deposited on one side of the planar flexible foam nickel substrate2A layer;
(3) chemical vapor deposition of a graphene network structure layer: transferring the planar flexible foamed nickel substrate with the SnO2 layer deposited by sputtering into a chemical vapor deposition device, and chemically vapor depositing a graphene net-shaped structure layer on the other side of the planar flexible foamed nickel substrate; the specific process parameters are as follows: the flow rate of methane is 20sccm, the flow rate of hydrogen is 40sccm, the flow rate of Ar is 40sccm, the reaction pressure is controlled to be 1Pa, and the deposition temperature is 300 ℃;
(4) bending into a three-layer composite cylindrical structure: will deposit SnO2Winding the planar flexible foam nickel substrate with the layer and the graphene net-shaped structure layer into a cylindrical structure, and bonding the gap with a conductive adhesive to obtain the planar flexible foam nickel substrate with the SnO inner layer2The composite structure comprises a layer, a middle layer and an outer layer, wherein the middle layer is a foam nickel substrate layer, and the outer layer is a three-layer composite cylindrical structure of a graphene net structure layer;
(5) connection of upper and lower electrodes: and (3) hermetically connecting the upper ends and the lower ends of a plurality of three-layer composite cylindrical structures which are arranged in a square array with the upper electrode and the lower electrode respectively.
Claims (6)
1. The three-layer cylindrical composite graphene-based hydrogen sensor comprises an upper electrode, a lower electrode and a middle composite structure positioned between the upper electrode and the lower electrode, and is characterized in that the middle composite structure is a three-layer composite cylindrical structure, and the inner layer of the three-layer composite cylindrical structure is SnO2The middle layer is a foam nickel substrate layer, the outer layer is a graphene net-shaped structure layer, the upper end of the three-layer composite cylindrical structure is connected with the upper electrode in a sealing mode, and the lower end of the three-layer composite cylindrical structure is connected with the lower electrode in a sealing modeSealing and connecting.
2. The three-layer cylindrical composite graphene-based hydrogen sensor according to claim 1, wherein: and a plurality of middle composite structures which are arranged in parallel are arranged between the upper electrode and the lower electrode and are connected with the upper electrode and the lower electrode in a parallel mode, so that the corresponding sensitivity of the hydrogen sensor to hydrogen is further improved.
3. The three-layer cylindrical composite graphene-based hydrogen sensor according to claim 2, wherein: the plurality of intermediate composite structures arranged in parallel are arranged in a single row in parallel, or in a cross-shaped array, or in a matrix in a shape of a Chinese character 'mi', or in a matrix in a shape of a Chinese character 'kou'.
4. The three-layer cylindrical composite graphene-based hydrogen sensor according to claim 1, wherein: the diameter of the three-layer composite cylindrical structure is 0.5mm-5mm, and the height of the three-layer composite cylindrical structure is 3mm-15 mm.
5. The three-layer cylindrical composite graphene-based hydrogen sensor according to claim 1, wherein: in the three-layer composite cylindrical structure, SnO2The thickness of the layer is 50nm-1 um; the thickness of the graphene net-shaped structure layer is 50nm-500 nm; the thickness of the foam nickel base layer is 20-100 um.
6. The preparation method of the three-layer cylindrical composite graphene-based hydrogen sensor according to any one of claims 1 to 5, comprising the following steps:
(1) pretreatment of a planar flexible foamed nickel substrate: taking planar flexible foamed nickel as a substrate, cleaning and pretreating the planar flexible foamed nickel, sequentially adopting ethanol, acetone and deionized water for ultrasonic cleaning, and then drying for later use;
(2) magnetron sputtering deposition of SnO2Layer (b): transferring the cleaned planar flexible foamed nickel serving as a matrix into a magnetron sputtering device, and using SnO2Ceramic materialThe target is a sputtering target, and SnO is obtained by reactive magnetron sputtering2A layer; the specific process parameters are as follows: background vacuum degree of 1X 10- 4Pa, 10% O by volume2The mixed gas of +90% Ar is sputtering gas, the sputtering pressure is 0.5-3Pa, the sputtering power is 200-400W, the sputtering time is 10-100min, and SnO is sputtered and deposited on one side of the planar flexible foamed nickel substrate2A layer;
(3) chemical vapor deposition of a graphene network structure layer: sputter deposited with SnO2Transferring the planar flexible foamed nickel substrate of the layer into a chemical vapor deposition device, and performing chemical vapor deposition on a graphene net-shaped structure layer on the other side of the planar flexible foamed nickel substrate; the specific process parameters are as follows: the flow rate of methane is 20-80sccm, the flow rate of hydrogen is 40-100sccm, the flow rate of Ar is 20-50sccm, the reaction pressure is controlled at 1-5Pa, the deposition temperature is 300-;
(4) bending into a three-layer composite cylindrical structure: winding the planar flexible foam nickel substrate deposited with the SnO2 layer and the graphene net-shaped structure layer into a cylindrical structure, and bonding the notches with conductive adhesive to obtain the planar flexible foam nickel substrate with the SnO2 layer as the inner layer2The composite structure comprises a layer, a middle layer and an outer layer, wherein the middle layer is a foam nickel substrate layer, and the outer layer is a three-layer composite cylindrical structure of a graphene net structure layer;
(5) connection of upper and lower electrodes: and (3) hermetically connecting the upper end and the lower end of the three-layer composite cylindrical structure with the upper electrode and the lower electrode respectively.
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