CN112946037A - Gas sensor and manufacturing method thereof - Google Patents
Gas sensor and manufacturing method thereof Download PDFInfo
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- CN112946037A CN112946037A CN202110354503.9A CN202110354503A CN112946037A CN 112946037 A CN112946037 A CN 112946037A CN 202110354503 A CN202110354503 A CN 202110354503A CN 112946037 A CN112946037 A CN 112946037A
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Abstract
The invention relates to the technical field of sensors, and provides a gas sensor and a manufacturing method thereof. The gas sensor comprises a substrate, a graphene layer, a metal electrode pair and a metal oxide layer; the substrate, the graphene layer and the metal electrode pairs are sequentially arranged from bottom to top; one metal electrode pair comprises two metal electrodes, and the region between the two metal electrodes of the one metal electrode pair is a channel; a gap groove is formed in the graphene layer at the channel, so that the graphene layer at the channel is disconnected to form a graphene electrode pair; the metal oxide layer is positioned at the channel and covers the graphene electrode pair and the clearance groove so as to be connected with the graphene electrode pair; the area of the metal oxide layer is smaller than that of the channel, so that the graphene layer which is not covered by the metal oxide layer but is exposed is arranged in the channel. The invention provides a gas sensor with high response strength and good response specificity and selectivity.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a gas sensor and a manufacturing method thereof.
Background
At present, more sensitive materials used by the gas sensor are mainly metal oxide layer semiconductors and organic semiconductor materials. The reaction between the traditional thick-film metal oxide layer semiconductor sensor and gas to be detected is very slow at room temperature, and the traditional thick-film metal oxide layer semiconductor sensor usually needs to be preheated and work at a higher temperature, for example, the SnO2 needs to be 70-350 ℃, the ZnO needs to be 300-450 ℃ and the like. The high operating temperature causes the impedance of the sensor to become very large, requiring more complex circuitry to be designed to avoid leakage. The organic semiconductor material has poor electrical and mechanical properties, and the function expansion of the organic semiconductor material on the high-performance gas sensor is limited due to the reasons of complex material preparation process, high cost and the like. As a typical two-dimensional material, graphene has characteristics of large specific surface area, extremely high carrier mobility, small intrinsic noise, easy chemical modification, flexibility, convenience for integration and the like, and has attractive application prospects in the fields of development of high-performance room-temperature gas sensors, particularly wearable equipment and the like. In a general graphene-based gas sensor, graphene mainly serves as a carrier material of a channel sensitive material, and a sensitive material, such as metal or metal oxide layer particles, mainly on the surface of graphene, which is sensitive to gas molecules, is generally consistent with the coverage area of the graphene carrier material.
However, the Sp2 hybrid orbital between the carbon atoms of graphene has a certain chemical inertness, so that the sensitivity of gas response is limited, the desorption process is slow, and the selectivity is poor. How to improve the response performance becomes a key point and a difficulty in the development of the graphene-based gas sensor. Some technical methods for improving the performance of the intrinsic graphene-based gas sensor are reported at present, such as increasing the working temperature of the sensor; or ozone treatment is carried out on the surface of the intrinsic graphene film to introduce oxygen-containing groups; or carrying out graphical processing on the graphene to increase the active position of gas adsorption; or modifying the substrate to which the graphene is attached, etc. The disadvantages of the above method are mainly high cost, poor stability, large power consumption, and not very good enhancement of sensor performance.
The Chinese invention patent publication No. CN109632906A (published as 2019, 04, 16) discloses a graphene-metal heterojunction-based gas sensor array and a preparation method thereof, wherein a resistance-type sensor of the patent comprises a metal electrode, a graphene film on the metal electrode and a metal covering layer on the top layer, the metal electrode comprises two electrode units, and the upper surfaces of the two electrode units are provided with continuous graphene films; the upper surface of the graphene film right above the two electrode unit gaps is provided with a metal covering layer, the top layer of the resistive sensor is provided with the metal covering layer, the covering layer completely covers the graphene above the two electrode unit gaps, on one hand, the graphene channel can be shielded, so that only the graphene-metal heterojunction is exposed outside, the response of the resistive sensor completely comes from the response of the graphene-metal heterojunction to gas, on the other hand, the metal covering layer and the graphene channel are in parallel connection in the measuring circuit, the proportion of the graphene film resistor in the total resistor is further reduced, and the response sensitivity of the heterojunction is improved. The patent only adopts a graphene film covered above a metal electrode as a sensitive material, and the gas response sensitivity of the patent is limited, the desorption process is slow, and the selectivity is poor because the step Sp2 hybridization orbit among graphene carbon atoms has certain chemical inertness.
Disclosure of Invention
The invention aims to provide a gas sensor with high response strength and good response specificity and selectivity and a manufacturing method thereof.
In order to achieve the above object, the present invention provides a gas sensor including a substrate, a graphene layer, a pair of metal electrodes, a metal oxide layer; the substrate, the graphene layer and the metal electrode pairs are sequentially arranged from bottom to top; one metal electrode pair comprises two metal electrodes, and the region between the two metal electrodes of the one metal electrode pair is a channel;
a gap groove is formed in the graphene layer at the channel, so that the graphene layer at the channel is disconnected to form a graphene electrode pair; the metal oxide layer is positioned at the channel and covers the graphene electrode pair and the clearance groove so as to be connected with the graphene electrode pair; the area of the metal oxide layer is smaller than that of the channel, so that the graphene layer which is not covered by the metal oxide layer but is exposed is arranged in the channel.
As a preferable scheme: the base plate comprises a silicon substrate and a silicon dioxide layer; the silicon dioxide layer is arranged on the silicon substrate, and the graphene layer is arranged above the silicon dioxide layer.
As a preferable scheme: the graphene electrode pairs are graphene interdigital electrode pairs; one graphene interdigital electrode pair comprises two comb-shaped graphene interdigital electrodes which are mutually staggered.
As a preferable scheme: the metal oxide layer is a native oxide layer of titanium or copper.
As a preferable scheme: the silicon dioxide layer is partially hollowed, and a metal electrode in contact with the silicon substrate is arranged in the hollowed area of the silicon dioxide layer to form a bottom electrode.
As a preferable scheme: the cross section of the metal electrode is rectangular; the side of the metal electrode pair close to the substrate is a chromium layer, and the side far away from the substrate is a gold layer.
As a preferable scheme: the thickness of the chromium layer is 3-8 nm, and the thickness of the gold layer is 6-10 nm; the width of the channel, namely the distance between two metal electrodes in one metal electrode pair is 1.5-2 mm.
As a preferable scheme: the thickness of the chromium layer is 8nm and the thickness of the gold layer is 8 nm.
The invention also provides a manufacturing method of the gas sensor, the manufacturing material comprises a substrate, and the method comprises the following steps:
step S1, preparing a graphene layer on the upper surface of the substrate;
step S2, manufacturing metal electrode pairs on the graphene layer, wherein a region between two metal electrodes of one metal electrode pair is a channel;
step S3, manufacturing the graphene layer at the channel into a graphene electrode pair;
step S4, depositing a metal material in the channel, so that the metal material covers the graphene electrode pairs to connect the graphene electrode pairs, and the area covered by the deposited metal material is smaller than the area of the channel, so that the graphene layer which is not covered by the metal material but is exposed is arranged in the channel; oxidizing the metal material to obtain a metal oxide layer to form a graphene-metal oxide heterojunction; and obtaining the gas sensor.
As a preferable scheme: the base plate comprises a silicon substrate and a silicon dioxide layer positioned above the silicon substrate, and in step S1, before the graphene layer is prepared, a metal alignment mark for photoetching is made on the base plate; removing the silicon dioxide layer of the local area on the surface of the substrate by an etching process, and depositing metal in the etched area to manufacture a bottom electrode; the substrate surface with the bottom electrode is cleaned.
Compared with the prior art, the invention has the beneficial effects that:
the invention arranges the metal electrode pairs on the graphene layer, covers the metal oxide layer with smaller area at the channel between the metal electrode pairs, leads the channel to have naked graphene, leads the graphene layer and the metal oxide layer to be two layers with completely different patterns, arranges the metal oxide layer and the graphene layer from top to bottom to form a graphene-metal oxide heterojunction, therefore, the graphene-metal oxide heterojunction and the naked graphene layer exist simultaneously, the graphene layer is used as a gas adsorption material and a conductive electrode of the sensor at the same time, the vertical electric field is conveniently loaded to modulate the barrier height of the graphene-metal oxide heterojunction, the response intensity and the response specificity are improved, the flexible modulation of the gas adsorption response intensity and the response selectivity with different attributes is realized, and the room-temperature detection of the gas is realized. In addition, the invention also provides a manufacturing method of the gas sensor.
Drawings
Fig. 1 is a plan view of a gas sensor according to embodiment 1 of the present invention.
Fig. 2 is a longitudinal sectional view of a gas sensor of embodiment 2 of the present invention.
Fig. 3 is a schematic flow chart of a method for manufacturing a gas sensor according to embodiment 2 of the present invention.
Wherein, 1-a substrate; 101-a silicon substrate; 102-a silicon dioxide layer; 2-a graphene layer; 3-a metal electrode; 301-gold layer; 302-a chromium layer; 4-a metal oxide layer; 5-a clearance groove; 6-graphene electrodes; 7-bottom electrode.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the description of the present invention, it should be noted that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In addition, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
Example 1
Specifically, as shown in fig. 1, the gas sensor of the present embodiment includes a substrate 1, a graphene layer 2, a metal electrode pair, and a metal oxide layer 4; the substrate 1, the graphene layer 2 and the metal electrode pairs are sequentially arranged from bottom to top; one metal electrode pair comprises two metal electrodes 3, and the region between the two metal electrodes 3 of the metal electrode pair is a channel;
the graphene layer 2 at the channel is provided with a clearance groove 5, so that the graphene layer 2 at the channel is disconnected to form a graphene electrode pair; the metal oxide layer 4 is located at the channel and covers the graphene electrode pair and the clearance groove 5 to connect the graphene electrode pair, and the metal oxide layer 4 of the embodiment covers the central area of the graphene electrode pair; the area of the metal oxide layer 4 is smaller than the area of the channel so that there is a graphene layer 2 inside the channel that is uncovered by the metal oxide layer 4. The metal oxide layer 4 is in contact with the graphene electrode pair and is vertically arranged to form a graphene-metal oxide heterojunction. The partial area of the graphene layer 2 at the channel is uncovered without being covered by the metal oxide layer 4, and the uncovered graphene electrode is used as a sensitive material of gas. Therefore, the graphene layer 2 is not only a conductive electrode of the sensor, but also serves as a material for gas adsorption, so that the modulation of the barrier height of the graphene-metal oxide heterojunction by loading a vertical electric field is facilitated, and the response intensity and the specific selectivity of the response are improved.
In the present embodiment, the base plate 1 includes a silicon substrate 101 and a silicon dioxide layer 102; the silicon dioxide layer 102 is arranged on the silicon substrate 101, the graphene layer 2 is arranged above the silicon dioxide layer 102, and the silicon dioxide layer 102 has insulating property and can ensure the conductivity of the graphene layer 2. The silicon substrate 101 of this embodiment is a heavily P-doped silicon substrate 101, so that the silicon substrate 101 has conductivity, and the thickness of the silicon dioxide layer 102 of this embodiment is 300 nm.
The graphene electrode pair of the embodiment is a graphene interdigital electrode pair; one graphene interdigital electrode pair comprises two comb-shaped graphene interdigital electrodes which are mutually staggered. And etching the graphene layer 2 between the metal electrode pairs into a clearance groove 5 by photoetching and inductively coupled oxygen plasma dry etching to manufacture the graphene interdigital electrode pair. The width of the gap trench 5 can be selected from 50-200 nm, which is 50nm in this embodiment. The graphene electrode pairs in the channel are manufactured into the interdigital electrode pairs, so that on one hand, better contact can be formed with the metal oxide layer 4, on the other hand, the number of active sites for gas molecule adsorption is greatly increased for the graphical edge defects introduced by the graphene layer 2, and therefore the response strength and response speed of the device to the gas molecules can be improved.
Optionally, the metal oxide layer 4 is a native oxide layer of titanium or copper, optionally a titanium dioxide layer or a copper oxide layer. Depositing a metallic material by photolithography and electron beam evaporation; the metal material comprises titanium Ti or copper Cu; the thickness of the metal material can be selected within the range of 5-10 nm, and the thickness of the metal material is 10nm in the embodiment; the metal material is deposited on the local surface of the graphene electrode pair and the local surface of the silicon dioxide layer 102, and the deposited metal material forms the metal oxide layer 4 through an ultrathin metal natural oxidation method, so that the oxidation method is convenient and efficient.
In addition, the silicon dioxide layer 102 is partially hollowed out, and a metal electrode 3 in contact with the silicon substrate 101 is arranged in the hollowed-out area of the silicon dioxide layer 102 to form a bottom electrode 7. The silicon dioxide layer 102 on the surface of the local area on the substrate is removed through an etching process, the silicon substrate 101 below the local area is exposed, and metal is deposited on the exposed area through a metal deposition process to manufacture the bottom electrode 7. Since the silicon substrate 101 is heavily doped, the conductivity is good, and the potential of the entire silicon substrate 101 can be controlled by the bottom electrode 7. The bottom electrode 7 is a structure independent of the device layout, and is an electrode formed in a predetermined region on the surface of the silicon substrate 101, and the shape thereof is determined according to the use requirement.
Alternatively, the cross-sectional shape of the metal electrode 3 is rectangular; the side of the metal electrode pair close to the substrate 1 is a chrome layer 302, and the side far away from the substrate 1 is a gold layer 301. Wherein the chrome layer 302 acts as an adhesion layer and the gold layer 301 acts as a main conductive structure for connection with external devices. In addition, the thickness of the chromium layer 302 is 3-8 nm, and the thickness of the gold layer 301 is 6-10 nm; the width of the channel, namely the distance between two metal electrodes 3 in one metal electrode pair is 1.5-2 mm. The thickness of the chrome layer 302 and the thickness of the gold layer 301 in this embodiment are 8nm and 8nm, respectively.
Example 2
Specifically, as shown in fig. 2 to 3, in the gas sensor of the present embodiment, the thickness of the silicon dioxide layer 102 of the present embodiment is 90 nm. The width of the gap trench 5 is 200nm in this embodiment. The metal oxide layer 4 is in this embodiment a copper oxide layer. Depositing a metallic material by photolithography and electron beam evaporation; the metal material thickness is 5nm in this example. The thickness of the chromium layer 302 and the thickness of the gold layer 301 in this embodiment are 3nm and 6nm, respectively. The spacing between the two metal electrodes 3 is 2mm in this example.
step S1, preparing a graphene layer 2 on the upper surface of the substrate 1;
step S2, manufacturing metal electrode pairs on the graphene layer 2, wherein a region between two metal electrodes 3 of one metal electrode pair is a channel;
step S3, manufacturing the graphene layer 2 at the channel into a graphene electrode pair;
step S4, depositing a metal material in the central area of the channel, covering the metal material on the graphene electrode pairs to connect the graphene electrode pairs, wherein the area covered by the deposited metal material is smaller than the area of the channel, and the graphene layer 2 which is not covered by the metal material but is exposed is arranged in the channel; oxidizing the metal material to obtain a metal oxide layer 43 to form a graphene-metal oxide heterojunction; and obtaining the gas sensor.
The generation method of the graphene layer 2 is a chemical vapor deposition method, and the single-layer rate of the graphene layer 2 is required to be more than 85%. The graphene layer 2 used in this embodiment is grown by chemical vapor deposition on a copper substrate, and then transferred onto the substrate 1. The graphene layer 2 with better quality can be obtained by using a chemical vapor deposition method, and the effective operation of the gas sensor is ensured.
The substrate 1 comprises a silicon substrate 101 and a silicon dioxide layer 102 positioned above the silicon substrate 101, and in step S1, before preparing the graphene layer 2, a metal alignment mark for lithography is made on the substrate 1; removing the silicon dioxide layer 102 on the local area of the surface of the substrate 1 by an etching process, and depositing metal on the etched area to manufacture a bottom electrode 7; the surface of the substrate 1 with the bottom electrode 7 is cleaned, and necessary preparation is performed for completion of the subsequent steps.
In step S2, a metal electrode pair is fabricated by photolithography and electron beam evaporation;
in step S4, a metal material is deposited by photolithography and electron beam evaporation;
in step S4, the metal oxide layer 4 is formed by an ultra-thin metal natural oxidation method;
to sum up, the embodiment of the present invention provides a gas sensor and a method for manufacturing the same, wherein a metal electrode pair is disposed on a graphene layer 2, a metal oxide layer 4 with a smaller area is covered at a channel between the metal electrode pair, so that bare graphene is disposed in the channel, the graphene layer 2 and the metal oxide layer 4 are structurally in two layers with completely different patterns, and the metal oxide layer 4 and the graphene layer 2 are disposed above and below to form a graphene-metal oxide heterojunction, therefore, the graphene-metal oxide heterojunction and the bare graphene layer 2 exist simultaneously, the graphene layer 2 is used as a material and a conductive electrode for gas adsorption of the sensor, the height of the graphene-metal oxide heterojunction barrier is conveniently modulated by loading a vertical electric field, the response strength and the specific selectivity of the response are improved, and the flexible modulation of the response strength and the response selectivity of gas adsorption with different properties is realized, the room temperature detection of the gas is realized. In addition, the invention also provides a manufacturing method of the gas sensor. In addition, the embodiment also provides a manufacturing method for manufacturing the gas sensor, which is convenient and efficient.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and substitutions can be made without departing from the technical principle of the present invention, and these modifications and substitutions should also be regarded as the protection scope of the present invention.
Claims (10)
1. A gas sensor, characterized by: the graphene-based graphene comprises a substrate (1), a graphene layer (2), a metal electrode pair and a metal oxide layer (4); the substrate (1), the graphene layer (2) and the metal electrode pair are sequentially arranged from bottom to top; one metal electrode pair comprises two metal electrodes (3), and the region between the two metal electrodes (3) of the one metal electrode pair is a channel;
a gap groove (5) is formed in the graphene layer (2) at the channel, so that the graphene layer (2) at the channel is disconnected to form a graphene electrode pair; the metal oxide layer (4) is positioned at the channel and covers the graphene electrode pair and the clearance groove (5) so as to be connected with the graphene electrode pair; the area of the metal oxide layer (4) is smaller than that of the channel, so that the graphene layer (2) uncovered by the metal oxide layer (4) is arranged in the channel.
2. The gas sensor according to claim 1, wherein: the substrate (1) comprises a silicon substrate (101) and a silicon dioxide layer (102); the silicon dioxide layer (102) is arranged on the silicon substrate (101), and the graphene layer (2) is arranged above the silicon dioxide layer (102).
3. The gas sensor according to claim 1, wherein: the graphene electrode pairs are graphene interdigital electrode pairs; one graphene interdigital electrode pair comprises two comb-shaped graphene interdigital electrodes which are mutually staggered.
4. The gas sensor according to claim 1, wherein: the metal oxide layer (4) comprises a native oxide layer of titanium or copper.
5. The gas sensor according to claim 2, wherein: further comprising a bottom electrode (7); the silicon dioxide layer (102) is partially hollowed, and a metal electrode (3) in contact with the silicon substrate (101) is arranged in the hollowed area of the silicon dioxide layer (102) to form the bottom electrode (7).
6. The gas sensor according to claim 1, wherein: the cross section of the metal electrode (3) is rectangular; one side of the metal electrode pair close to the substrate (1) is a chromium layer (302), and one side far away from the substrate (1) is a gold layer (301).
7. The gas sensor according to claim 6, wherein: the thickness of the chromium layer (302) is 3-8 nm, and the thickness of the gold layer (301) is 6-10 nm; the width of the channel, namely the distance between two metal electrodes (3) in one metal electrode pair is 1.5-2 mm.
8. The gas sensor according to claim 7, wherein: the thickness of the chromium layer (302) is 8nm, and the thickness of the gold layer (301) is 8 nm.
9. A method for manufacturing a gas sensor, the manufacturing material comprising a substrate (1), characterized by comprising the steps of:
step S1, preparing a graphene layer (2) on the upper surface of the substrate (1);
step S2, manufacturing metal electrode pairs on the graphene layer (2), wherein a region between two metal electrodes (3) of one metal electrode pair is a channel;
step S3, manufacturing the graphene layer (2) at the channel into a graphene electrode pair;
step S4, depositing a metal material in the channel, enabling the metal material to cover the graphene electrode pairs to be connected with the graphene electrode pairs, enabling the area covered by the deposited metal material to be smaller than the area of the channel, and enabling the graphene layer (2) uncovered by the metal material to be arranged in the channel; oxidizing the metal material to obtain a metal oxide layer (4) and forming a graphene-metal oxide heterojunction; and obtaining the gas sensor.
10. The method of manufacturing a gas sensor according to claim 9, wherein: the substrate (1) comprises a silicon substrate (101) and a silicon dioxide layer (102) positioned above the silicon substrate (101), and in step S1, before the graphene layer (2) is prepared, a metal alignment mark for lithography is made on the substrate (1); removing the silicon dioxide layer (102) in a local area on the surface of the substrate (1) through an etching process, and depositing metal in the etched area to manufacture a bottom electrode (7); cleaning the surface of the substrate (1) with the bottom electrode (7).
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113533300A (en) * | 2021-07-22 | 2021-10-22 | 岭南师范学院 | Graphene plasmon gas sensor and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113533300A (en) * | 2021-07-22 | 2021-10-22 | 岭南师范学院 | Graphene plasmon gas sensor and manufacturing method thereof |
| CN113533300B (en) * | 2021-07-22 | 2022-06-21 | 岭南师范学院 | Graphene plasmon gas sensor and manufacturing method thereof |
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