CN111584682A - Flexible optical detection device based on graphene and manufacturing method thereof - Google Patents

Flexible optical detection device based on graphene and manufacturing method thereof Download PDF

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CN111584682A
CN111584682A CN202010405762.5A CN202010405762A CN111584682A CN 111584682 A CN111584682 A CN 111584682A CN 202010405762 A CN202010405762 A CN 202010405762A CN 111584682 A CN111584682 A CN 111584682A
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graphene
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CN111584682B (en
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冯雪
孟艳芳
马寅佶
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Tsinghua University
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Abstract

The present disclosure relates to a flexible optical detection device based on graphene and a method for manufacturing the same. The method comprises the steps of preparing single-layer graphene, preparing a first metal electrode and a second metal electrode on a flexible substrate, manufacturing n-type graphene and p-type graphene, and manufacturing a transparent grid layer. According to the graphene-based flexible optical detection device and the manufacturing method thereof, the processing process of the manufacturing device is simple. The manufacture of the device is realized by using the same semiconductor, so that the manufacture efficiency of the device is high, the cost is low, and the problems of interface and lattice mismatch in the related art are solved. The manufactured device has good mechanical property, good chemical resistance, acid resistance and alkali resistance, improves the durability, stability and reliability of the device, has flexibility and is suitable for the field of flexible electronics.

Description

Flexible optical detection device based on graphene and manufacturing method thereof
Technical Field
The present disclosure relates to the field of flexible electronic technologies, and in particular, to a flexible optical detection device based on graphene and a manufacturing method thereof.
Background
Photodetectors are powerful electronic devices based on radiation causing a change in the conductivity of an illuminated material. The method has wide application, and is mainly used for ray measurement and detection, industrial automatic control, photometric measurement and the like in visible light or near infrared bands; the infrared band is mainly used for missile guidance, infrared thermal imaging, infrared remote sensing and the like. It can be divided into: phototubes, photoresistors, photodiodes, photomultiplier tubes, photocells, quad limit detectors, thermocouples, thermistors, pyroelectric detectors, and the like. The principle of the method is divided into an external photoelectric effect and an internal photoelectric effect. The internal photoelectric effect is further classified into a photoconductive effect and a photovoltaic effect. The external photoelectric effect refers to a phenomenon that electrons in an object escape from the surface of the object and are emitted outwards under the action of light, and is mostly generated in materials such as metal, metal oxide and the like. The internal photoelectric effect is a phenomenon that when light is irradiated on an object, the resistivity of the object changes or a photo-generated electromotive force is generated, and is often generated in a semiconductor.
A photodetector based on a semiconductor heterojunction type is composed of a p-type semiconductor and an n-type semiconductor, and has been a focus of recent research due to its advantages such as angular selectivity of light absorption, broad-band absorption in a wide wavelength range, controllability, and the like. Important parameters of the photodetector are the degree of detection and the sensitivity. At present, the optical detector based on high perovskite absorptivity, long free path of a carrier, difficult recombination and long service life attracts the most attention. However, the poor stability of the perovskite and the solvent intolerance limit its application. Thus, graphene-based photodetectors are an alternative choice in the related art. However, since the graphene carbon semiconductor has a 0 band gap and no photovoltaic effect, the graphene carbon semiconductor generally needs to be assembled with other materials to realize a light detection function. Although the sensitivity and the detection degree are greatly improved, the optical detector is complex to process, low in efficiency and high in cost. And the manufactured optical detector has high hardness and is difficult to adapt to the use requirement in the field of flexible electronics at the present stage.
Disclosure of Invention
In view of this, the present disclosure provides a flexible optical detection device based on graphene and a manufacturing method thereof.
According to an aspect of the present disclosure, there is provided a method for manufacturing a flexible graphene-based optical detection device, the method including:
etching a metal layer prepared in advance according to a preset shape to obtain an etched metal layer, wherein the etched metal layer is provided with a fixing part;
growing a first single-layer graphene on the etched metal layer fixed by the fixing part in a chemical vapor deposition mode;
after a temporary substrate layer is prepared on the first single-layer graphene, removing the etched metal layer;
transferring the first single-layer graphene with the temporary substrate layer to a first metal electrode on a pre-prepared flexible substrate, and removing the temporary substrate layer;
selectively doping the first single-layer graphene to obtain doped graphene;
placing pre-prepared undoped single-layer graphene on a second metal electrode on the flexible substrate, wherein a contact area exists between the undoped single-layer graphene and the doped graphene;
and preparing a transparent grid layer on the top of the device, wherein a part of region of the transparent grid layer covers the position, corresponding to the contact region, on the undoped single-layer graphene, so as to obtain the flexible light detection device.
In one possible implementation manner, growing a first single-layer graphene on the etched metal layer by using a chemical vapor deposition method includes:
after the etched metal layer is fixedly placed in a vacuum quartz tube by using the fixing part, pressurizing the quartz tube to a preset pressure, introducing hydrogen, heating to a first temperature, and keeping the first temperature for a first time;
continuously introducing hydrogen into the quartz tube at a first flow rate, and simultaneously introducing methane gas at a second flow rate, so that graphene grows on the etched metal layer;
and stopping introducing the methane gas after the duration of keeping the introducing states of the hydrogen gas and the methane gas reaches a second duration, so as to obtain the etched metal layer with the first single-layer graphene.
In one possible implementation manner, selectively doping the first single-layer graphene to obtain a doped graphene includes:
placing a bearing part with a protrusion on a region to be doped of the first single-layer graphene, wherein only the protrusion in the bearing part is in contact with the region to be doped of the first single-layer graphene, and a solution to be doped is coated on the protrusion;
and applying pressure to the bearing part to enable the solution to be doped to dope the first single-layer graphene so as to obtain doped graphene.
In one possible implementation, the shape of the load bearing member comprises a pyramidal shape,
when the bearing part is in the pyramid shape, the top of the pyramid shape serves as the protrusion.
In one possible implementation, the method further includes:
preparing an electrode metal layer on a flexible substrate;
etching the electrode metal layer to form a first metal electrode and a second metal electrode to obtain a flexible substrate with the first metal electrode and the second metal electrode,
wherein a space exists between the first metal electrode and the second metal electrode.
In one possible implementation, the method further includes:
before selectively doping the first single-layer graphene, etching the first single-layer graphene, so that part of the etched first single-layer graphene covers the first metal electrode, and the other part of the etched first single-layer graphene is suspended among the intervals.
In one possible implementation, after preparing a temporary substrate layer on the first single-layer graphene, removing the etched metal layer includes:
and removing the etched metal layer by using a removing liquid which only reacts with the etched metal layer.
In one possible implementation, preparing a transparent gate layer on top of the device includes:
placing a liquid fence around the flexible substrate to form a bearing groove;
after the ionic gel liquid is added into the bearing groove, exposing the ionic gel liquid according to a preset pattern shape, so that polymerization reaction required for forming a transparent gate layer is generated at the exposed position in the ionic gel liquid;
and removing the unexposed ionic gel liquid on the flexible substrate to obtain the transparent gate layer.
In one possible implementation, the method further includes:
and filling an insulating substance in the space between the first metal electrode and the second metal electrode.
According to an aspect of the present disclosure, there is provided a graphene-based flexible optical detection device, the device being manufactured by the above method, the device including: a flexible substrate, a first metal electrode, a second metal electrode, doped graphene, undoped monolayer graphene and a transparent gate layer,
the first metal electrode and the second metal electrode are positioned on the flexible substrate, and a gap is formed between the first metal electrode and the second metal electrode;
the doped graphene part is positioned on the first metal electrode, and the other part is positioned between the intervals;
the undoped single-layer graphene is positioned on the second metal electrode, and a contact area exists between the undoped single-layer graphene and the doped graphene;
the transparent gate layer is positioned on the top of the device, and a partial region of the transparent gate layer covers a position corresponding to the contact region on the undoped single-layer graphene.
According to the graphene-based flexible optical detection device and the manufacturing method thereof, the processing process of the manufacturing device is simple. The manufacture of the device is realized by using the same semiconductor, so that the manufacture efficiency of the device is high, the cost is low, and the problems of interface and lattice mismatch in the related art are solved. The manufactured device has good mechanical property, good chemical resistance, acid resistance and alkali resistance, improves the durability, stability and reliability of the device, has flexibility and is suitable for the field of flexible electronics.
Other features and aspects of the present disclosure will become apparent from the following detailed description of exemplary embodiments, which proceeds with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate exemplary embodiments, features, and aspects of the disclosure and, together with the description, serve to explain the principles of the disclosure.
Fig. 1 shows a flowchart of a method of manufacturing a graphene-based flexible light detection device according to an embodiment of the present disclosure.
Fig. 2a, 2b, and 2c are schematic structural diagrams illustrating a flexible light detection device based on graphene according to an embodiment of the present disclosure.
Fig. 3a shows the output curves of a p-type photo-detection device at different gate voltages.
Fig. 3b shows the transfer curves of a p-type photo-detection device at different gate voltages.
Fig. 4a shows the output curves of an n-type photo-detection device at different gate voltages.
Fig. 4b shows the transfer curves of an n-type photo-detection device at different gate voltages.
Figure 5 shows the photodetector performance of the photodetecting device as a homogeneous semiconductor heterojunction.
Detailed Description
Various exemplary embodiments, features and aspects of the present disclosure will be described in detail below with reference to the accompanying drawings. In the drawings, like reference numbers can indicate functionally identical or similar elements. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
Furthermore, in the following detailed description, numerous specific details are set forth in order to provide a better understanding of the present disclosure. It will be understood by those skilled in the art that the present disclosure may be practiced without some of these specific details. In some instances, methods, means, elements and circuits that are well known to those skilled in the art have not been described in detail so as not to obscure the present disclosure.
Fig. 1 shows a flowchart of a method of manufacturing a graphene-based flexible light detection device according to an embodiment of the present disclosure. Fig. 2a, 2b, and 2c are schematic structural diagrams illustrating a flexible light detection device based on graphene according to an embodiment of the present disclosure. Fig. 2a, 2b, 2c show examples of devices manufactured according to the manufacturing method given in fig. 1. Fig. 2a is a front view of the device, fig. 2b is a cross-sectional view of the device taken along line ab in fig. 2a, and fig. 2c is a top view of the device.
As shown in fig. 1, the method includes steps S11 through S17.
In step S11, etching the metal layer prepared in advance according to a preset shape to obtain an etched metal layer, where the etched metal layer has a fixing portion.
In this embodiment, a piranha etching solution (H) can be used for the etched metal layer2SO4And H2O2Mixing the above two solutions at a ratio of 7:3), cleaning with surface impurities, further cleaning with deionized water, and drying with hydrogen gas. The etching of the metal layer may be accomplished using a photolithography process, which is not limited by this disclosure. The material of the metal layer may be copper, nickel, or other metal that catalyzes the growth of graphene and is easily removed by etching later, which is not limited by the present disclosure.
In step S12, a first single layer of graphene is grown on the etched metal layer fixed by the fixing portion by Chemical Vapor Deposition (CVD). Therefore, the preparation of the single-layer graphene is realized through the CVD process, the high quality and the area of the prepared single-layer graphene can be ensured to meet the use requirements of different types of optical detection devices, and the single-layer graphene grows on the etched metal layer, so that the transfer and assembly of the single-layer graphene in the subsequent steps are facilitated.
In one possible implementation, step S12 may include:
after the etched metal layer is fixedly placed in a vacuum quartz tube by using the fixing part, pressurizing the quartz tube to a preset pressure, introducing hydrogen, heating to a first temperature, and keeping the first temperature for a first time;
continuously introducing hydrogen into the quartz tube at a first flow rate, and simultaneously introducing methane gas at a second flow rate, so that graphene grows on the etched metal layer;
and stopping introducing the methane gas after the duration of keeping the introducing states of the hydrogen gas and the methane gas reaches a second duration, so as to obtain the etched metal layer with the first single-layer graphene.
In the implementation mode, the etched metal layer can be placed in other spaces which can realize vacuum and ensure the normal operation of the synthesis process of the graphene. The etched metal layer can be fixed in the quartz tube by using a weight which can press the fixing part to ensure that the etched metal layer does not move in the process of introducing hydrogen and methane. Or, the fixing part and the edge of the quartz tube can be clamped and fixed together by utilizing the clamping part, so that the metal layer is fixed after etching. The method for fixing the etched metal layer can be set by a person skilled in the art according to actual needs, and the disclosure does not limit this.
In this implementation, the preset pressure, the first flow rate, the second flow rate, the first time duration, and the second time duration may be set according to the size and the quality of the single-layer graphene, which is not limited by the present disclosure.
In step S13, after a temporary substrate layer is prepared on the first single-layer graphene, the etched metal layer is removed.
In this embodiment, the material of the temporary substrate layer may be a flexible material such as polymethyl methacrylate (PMMA), polyethylene terephthalate (PET), Polyimide (PI), and the disclosure is not limited thereto. The temporary substrate layer can be prepared by using adaptive methods such as spin coating and drop coating according to different materials of the temporary substrate layer, for example, a PMMA solution can be directly spin-coated on the first single-layer graphene, or a chlorobenzene solution of PMMA can be directly spin-coated on the first single-layer graphene.
In one possible implementation, step S13 may include: and removing the etched metal layer by using a removing liquid which only reacts with the etched metal layer.
In the implementation mode, because the first single-layer graphene is grown and prepared on the etched metal layer, the etched metal layer can be removed by using the removing liquid which can only react with the etched metal layer, so that the removing process of the etched metal layer can be simplified, and adverse effects on graphene in the process of removing the grown graphene carrier in the traditional mode in an etching mode can be avoided (for example, the graphene is easily damaged in the mode of excessively soft etching, cracks and the like). For example, if the material of the etched metal layer is copper, the material may be removed by using a solution of ammonium persulfate, and the "temporary substrate-first single-layer graphene-etched metal layer" structure is placed in a solution of ammonium persulfate, and after it is determined that the etched metal layer is dissolved, the ammonium persulfate attached to the surface of the remaining "temporary substrate-first single-layer graphene" is washed away.
In step S14, the first single-layer graphene with the temporary substrate layer is transferred onto a first metal electrode on a pre-prepared flexible substrate, and the temporary substrate layer is removed.
In this embodiment, the first single-layer graphene with the temporary substrate layer may be directly transferred onto the first metal electrode by using a clamping transfer apparatus, and a person skilled in the art may set a transfer mode according to actual needs, which is not limited in this disclosure. The material of the flexible substrate may be flexible, malleable, and in the operating state of the device, such as Polyethylene terephthalate (PET or PEIT), Polyimide (PI), and the like.
In this embodiment, the temporary substrate layer can be removed using a solution that can react with the temporary substrate layer to release it from the first monolayer graphene. For example, where the material of the temporary substrate layer is PMMA, the PMMA may be removed with acetone.
In one possible implementation, before step S14, the method may further include:
preparing an electrode metal layer on a flexible substrate;
etching the electrode metal layer to form a first metal electrode and a second metal electrode to obtain a flexible substrate with the first metal electrode and the second metal electrode,
wherein a space exists between the first metal electrode and the second metal electrode.
In this implementation, the flexible substrate that has been prepared may be first surface cleaned, for example, by placing it in acetone, isopropanol and deionized water for 5min of ultrasonic cleaning. And then, an electrode metal layer is manufactured on the flexible substrate in an evaporation mode, and the heating mode of evaporation can be selected according to the material of the electrode metal layer. The electrode metal layer can be made of metal materials with good flexibility, extensibility and electrical conductivity, such as gold and copper. After the preparation of the metal electrode layer is completed, the metal electrode layer can be etched by using etching techniques such as photolithography and the like to form a first metal electrode and a second metal electrode. For example, when the material of the electrode metal layer is gold, the electrode metal layer can be etched by using an ultraviolet exposure machine. Specifically, the photoresist may be spin-coated on the electrode metal layer, and then the processes of uv exposure, development, and etching are performed to obtain the first metal electrode and the second metal electrode.
In this implementation, the spacing between the first metal electrode and the second metal electrode may be set according to the design requirements of the device, which is not limited by the present disclosure.
In this implementation manner, before the electrode metal layer is prepared on the flexible substrate, an auxiliary metal layer may be prepared on the flexible substrate in advance, and then the electrode metal layer is prepared on the auxiliary metal layer. And then respectively etching the electrode metal layer and the auxiliary metal layer to obtain a first metal electrode and a second metal electrode, wherein the auxiliary metal layer with the shape (similar or identical) to that of the first metal electrode is arranged between the first metal electrode and the flexible substrate, and the auxiliary metal layer with the shape (similar or identical) to that of the second metal electrode is arranged between the second metal electrode and the flexible substrate. The auxiliary metal layer is used for enhancing the adhesion between the first metal electrode and the flexible substrate and between the second metal electrode and the flexible substrate, and ensuring that the first metal electrode and the second metal electrode are stably fixed on the flexible substrate. The material of the auxiliary metal layer can be a metal material with good adhesion to the flexible substrate material and good adhesion to the material of the metal electrode layer, such as chromium. The thickness of the auxiliary metal layer can be set according to the thickness of the electrode metal layer and the flexible substrate, and for example, the thickness of the auxiliary metal layer can be 7nm-10 nm.
In one possible implementation, the method may further include: and filling an insulating substance in the space between the first metal electrode and the second metal electrode.
In this implementation, as shown in fig. 2a, since the doped graphene is suspended in the gap, although the single-layer graphene can meet the normal detection requirement in the suspended state, in order to further ensure the stability of the device structure, an insulating material may be filled between the first metal electrode and the second metal electrode.
In one possible implementation, before step S15, the method further includes:
before selectively doping the first single-layer graphene, etching the first single-layer graphene, so that part of the etched first single-layer graphene covers the first metal electrode, and the other part of the etched first single-layer graphene is suspended among the intervals.
In this implementation manner, since the first single-layer graphene directly transferred to the first metal electrode has a large size and is not accurately operated in the transfer process, the first single-layer graphene can be etched by photolithography and the like, so that the size assembly requirement of the device on the first single-layer graphene can be met.
In step S15, the first single-layer graphene is selectively doped to obtain doped graphene.
In one possible implementation, step S15 may include:
placing a bearing part with a protrusion on a region to be doped of the first single-layer graphene, wherein only the protrusion in the bearing part is in contact with the region to be doped of the first single-layer graphene, and a solution to be doped is coated on the protrusion;
and applying pressure to the bearing part to enable the solution to be doped to dope the first single-layer graphene so as to obtain doped graphene.
In one possible implementation, the shape of the load bearing member comprises a pyramidal shape,
when the bearing part is in the pyramid shape, the top of the pyramid shape serves as the protrusion.
In the implementation mode, the bearing part with the bulge is used for doping, the bulge can be arranged according to the size of the region to be doped, and the doping accuracy is ensured. Meanwhile, the pressure is applied to the bearing part, so that the doping process can be accelerated. The bearing part can be provided with a bulge, the region corresponding to the bulge is doped every time, and doped graphene is obtained after multiple times of doping. The size of the contact part of the protrusion and the graphene can be directly set to be consistent with that of the region to be doped, so that the doping process can be realized at one time. In mass production, a plurality of protrusions can be provided, while the doping of a plurality of first monolayer graphene is achieved.
In this implementation manner, the solution to be doped may be a Polyetherimide (PEI for short) solution or the like that can dope graphene, which is not limited in this disclosure. The material of the bearing part can be flexible material such as polydimethylsiloxane (PDMS for short), so that normal doping can be ensured, and damage to graphene due to hard texture of the bearing part can be avoided.
In this implementation, a pressure may also be applied to the region to be doped of the first single-layer graphene to facilitate doping, which is not limited by the present disclosure.
In step S16, pre-prepared undoped single-layer graphene is placed on a second metal electrode on the flexible substrate, and a contact region exists between the undoped single-layer graphene and the doped graphene.
In this embodiment, the undoped single-layer graphene can be manufactured by referring to the process of preparing the first single-layer graphene, and details are not repeated here. The size of the undoped single-layer graphene placed on the second metal electrode can be the size which meets the requirements of the device, or the size which is larger than the requirements of the device. When the size of the undoped single-layer graphene is larger and does not meet the requirement of the device, the first single-layer graphene can be etched in the same manner, so that the size of the first single-layer graphene meets the requirement.
In step S17, a transparent gate layer on top of the device is prepared, and a partial region of the transparent gate layer covers a position corresponding to the contact region on the undoped single-layer graphene, so as to obtain the flexible light detection device.
Wherein the transparent gate layer is the device gate. After the device is manufactured, the device is required to be tested, whether the device is qualified or not is determined according to the testing process and the result, and a source electrode and a drain electrode of the device are determined, wherein one of the first metal electrode and the second metal electrode is the drain electrode, and the other one is the source electrode.
In this embodiment, the transparent gate layer covers the flexible substrate except for the portion covering the contact region, and the size of the portion covering the flexible substrate may be set according to the size requirement of the device gate.
In one possible implementation, step S17 may include:
placing a liquid fence around the flexible substrate to form a bearing groove;
after the ionic gel liquid is added into the bearing groove, exposing the ionic gel liquid according to a preset pattern shape, so that polymerization reaction required for forming a transparent gate layer is generated at the exposed position in the ionic gel liquid;
and removing the unexposed ionic gel liquid on the flexible substrate to obtain the transparent gate layer.
In this implementation, the high molecular organic polymer in the ionic gel liquid and the salt electrolyte that can be electrolyzed into ions may be set according to the design requirements of the transparent gate layer, which is not limited by the present disclosure. The liquid fence can be placed around the flexible substrate by using transparent adhesive tape, prefabricated strip-shaped film and the like to form a bearing groove, so that the ionic gel liquid can be loaded in the bearing groove. Alternatively, a carrier groove capable of placing the flexible substrate may be prepared in advance, and then the flexible substrate may be directly placed in the carrier groove.
For example, the ionic gel liquid may be a mixture of ionic liquid 1-ethyl-3-methylimidazole-bis (trifluoromethylsulfonate) imidazole (EMIM-TFSI), monomeric polyethylene glycol diacrylate monomer (PEG-DA), and photoinitiator 2-methyl propylphenone (HOMPP) in a specified mass ratio (e.g., 90:8: 2). The ionic gel liquid may be exposed through the prepared template for a set time (e.g., 10 seconds) under ultraviolet light. Under ultraviolet light, an initiator HOMPP generates free radicals to react with PEG-DA, and the polymerization of monomer PEG-DA is initiated. The ionic gel liquid not exposed to light has no polymerization reaction and can be washed away with deionized water or the like.
In this embodiment, since the doped graphene is n-type graphene below, and the undoped single-layer graphene is p-type graphene above, the manufactured device is a p-type optical detection device. Based on the same manufacturing process, the n-type optical detection device can be manufactured by doping the n-type graphene on the doped graphene and doping the p-type graphene on the undoped single-layer graphene, and the manufacturing process of the n-type optical detection device is different from that of the p-type optical detection device only in the upper and lower positions of the p-type graphene and the n-type graphene, so that the n-type optical detection device can be manufactured by referring to the manufacturing process of the p-type optical detection device, and the details are not repeated herein.
According to the manufacturing method of the flexible optical detection device based on the graphene, the processing process of the manufacturing device is simple. The manufacture of the device is realized by using the same semiconductor, so that the manufacture efficiency of the device is high, the cost is low, and the problems of interface and lattice mismatch in the related art are solved. The manufactured device has good mechanical property, good chemical resistance, acid resistance and alkali resistance, improves the durability, stability and reliability of the device, has flexibility and is suitable for the field of flexible electronics.
The manufacturing method can be used for manufacturing the light detection device, and the light detection device comprises the following steps: a flexible substrate 1, a first metal electrode 2, a second metal electrode 3, doped graphene 4, undoped single-layer graphene 5 and a transparent gate layer 6,
the first metal electrode 2 and the second metal electrode 3 are positioned on the flexible substrate 1, and a space exists between the first metal electrode 2 and the second metal electrode 3;
part of the doped graphene 5 is positioned on the first metal electrode 2, and the other part of the doped graphene is positioned between the intervals;
the undoped single-layer graphene 4 is positioned on the second metal electrode 3, and a contact area exists between the undoped single-layer graphene 4 and the doped graphene 5;
the transparent gate layer 6 is located on top of the device, and a partial region of the transparent gate layer 6 covers a position on the undoped single-layer graphene 4 corresponding to the contact region.
In this embodiment, the flexible substrate 1 may have a length of 1cm to 3cm, a width of 1cm to 3cm, and a thickness of 4mm to 6mm (e.g., 5 mm). The length and width of the transparent grid layer 6 and the area covering the flexible substrate part can be 2mm-4mm, the thickness can be 400 μm-1000 μm, the length of the area covering the contact area with graphene can be 280 μm-980 μm, the width can be 100 μm-150 μm, and the thickness of the area covering the flexible substrate part is different from the sum of the thicknesses of the second metal electrode, the undoped single-layer graphene and the doped graphene. The first metal electrode may have a thickness of 40nm to 100nm, a length of 1mm to 2mm, and a width of 100 μm to 200 μm. The length of the second metal electrode can also be 1mm-2mm, the width can also be 100 μm-200 μm, and the thickness is the sum of the thickness of the first metal electrode and the thickness of the doped graphene. The width of the space between the first metal electrode and the second metal electrode may be 300 μm to 1000 μm. The width of the doped graphene can be 100-200 μm, and the length can be set according to the length of the first metal electrode, the length of the second metal electrode, and the spacing width between the first metal electrode and the second metal electrode.
To further clarify the implementation of the manufacturing method provided by the present disclosure, the following describes the manufacturing of the graphene-based optical detection device as shown in fig. 2a, fig. 2b, and fig. 2c by way of an example. It is to be understood by those skilled in the art that the following examples are for the purpose of facilitating understanding of the embodiments of the present disclosure only and are not to be construed as limiting the embodiments of the present disclosure. The specific manufacturing process is as follows:
preparing single-layer graphene:
firstly, etching a copper foil (namely a metal layer) with the thickness of 25 mu m to obtain an etched copper foil with the area capable of growing graphene at least being 10cm multiplied by 10cm, wherein the etched copper foil is provided with a fixing part. And then cleaning the etched copper foil for 15min by using piranha solution. Finally, the etched copper foil is soaked in deionized water to remove piranha solution, and then is dried by nitrogen.
Then, the etched copper foil was fixed in a vacuum quartz tube by a fixing portion, and then it was introduced into a quartz tube which was exhausted of air, when the internal pressure of the quartz tube reached 5 × 10-3While the pressure was Torr (i.e., the preset pressure), H2 was introduced while the quartz tube was heated to 1000 deg.C (i.e., the first temperature) for 30min (i.e., the first period). At a first flow rate of 10sccm (10sccm representing one atmosphere at 25 ℃ C., 1 cubic centimeter (or milliliter) per minute (i.e., 1ml/min or 1 cm)3Flow rate per min)) was continuously fed in H2While introducing a second stream at a flow rate of 5sccmFast) CH4Gas, causing graphene to grow continuously on the copper foil. Sustained H2、CH4After 30min (i.e. the second period of time), the CH introduction was stopped4So that the quartz tube is at H2Cooling the stream to room temperature to obtain the first monolayer graphene grown on the copper foil. A second single layer of graphene was prepared on another copper foil based on the same procedure.
Preparing a first metal electrode and a second metal electrode on a flexible substrate:
the flexible substrate 1 was ultrasonically cleaned in acetone, isopropanol and deionized water for 5 min. And (3) evaporating chromium with the thickness of 7nm-10nm and gold with the thickness of 50nm-70nm on the flexible substrate 1 by a thermal evaporation method to obtain an auxiliary metal layer and an electrode metal layer. And photoetching the electrode metal layer and the auxiliary metal layer by using an ultraviolet exposure machine to obtain a source electrode (or a drain electrode) of the first metal electrode 2 device and a drain electrode (or a source electrode) of the second metal electrode 3 device, wherein intervals are arranged between the first metal electrode 2 and the second metal electrode 3, and the auxiliary metal layer chromium is arranged between the first metal electrode 2 and the flexible substrate 1 and between the second metal electrode 3 and the flexible substrate 2.
Manufacturing n-type graphene and p-type graphene:
spin coating a PMMA solution (mass fraction of 4.6%) on the first single-layer graphene at a rotation speed of 3000 rpm/sec for 1min to obtain a temporary substrate layer. And then placing the copper foil-first single-layer graphene-temporary substrate layer structure in a solution of ammonium persulfate to enable the copper foil-first single-layer graphene-temporary substrate layer structure to be suspended. After the copper foil is dissolved, transferring the copper foil to clean water to wash away residual ammonium persulfate solution, finally transferring the 'first single-layer graphene-temporary substrate layer' to the flexible substrate 1, and removing the temporary substrate layer on the first single-layer graphene by using acetone after drying. And then, photoetching the first single-layer graphene by using an ultraviolet exposure machine to enable the size of the first single-layer graphene to meet the manufacturing requirement.
Subsequently, an ethanol solution (i.e., a solution to be doped) of PEI with a mole fraction of 40mmol/L (molecular weight: 10000) was spin-coated on the top (i.e., the bumps) of the support with the pyramid-type microstructure at 3000rpm for 1 min. And then, under a microscope, applying pressure to a region to be doped of the first single-layer graphene, and selectively doping the first single-layer graphene to obtain doped graphene 5, wherein the doped graphene 5 is n-type graphene.
Then, the second single-layer graphene on the other copper foil is transferred to the second metal electrode 3 (the position is as described above), and then the second single-layer graphene is photoetched by using an ultraviolet exposure machine, so that the size of the second single-layer graphene meets the manufacturing requirement, and the undoped single-layer graphene 4 is obtained, wherein the undoped single-layer graphene 4 is p-type graphene.
Thus, a structure in which p-type graphene is on top and n-type graphene is on bottom is formed.
Manufacturing a transparent grid layer:
surrounding the periphery of the flexible substrate 1 by using a transparent adhesive tape to form a carrying groove, then pouring the ionic gel liquid into the carrying groove, and exposing for 10 seconds through a template (the hollow pattern shape of the template is the same as the overlooking shape of the transparent gate layer in fig. 2 c) under ultraviolet light, so that the exposed position in the ionic gel liquid generates polymerization reaction required for forming the transparent gate layer. The unexposed ionic gel liquid is then removed with deionized water to yield transparent gate layer 6.
At this time, the entire p-type photodetector device is completed. Based on a similar process, an n-type photo-detection device can also be manufactured.
The present disclosure also examined the p-type optical detection device and the n-type optical detection device manufactured by the above examples.
Fig. 3a shows the output curves of a p-type photo-detection device at different gate voltages. As shown in fig. 3a, it shows that the source-drain current and the source-drain voltage present a better linear relationship, and there is no saturation region, which represents half-metallic graphene. Meanwhile, the absolute value of the source-drain current increases along with the increase of the absolute value of the grid voltage, which shows that the larger the grid voltage is, the more obvious the regulation and control of the carrier transmission of the device are. When the source-drain voltage is fixed at 0.5V, the absolute value of the gate voltage is increased from 0V to-2V, and the absolute value of the source-drain current is increased from 2.57 muA to 19.10 muA. Fig. 3b shows the transfer curves of a p-type photo-detection device at different gate voltages. As shown in fig. 3b, the curve is approximately parabolic in shape, indicating that the device is bipolar in transmission characteristics; and the operating voltage can be regulated and controlled only at 2V, which shows that the larger capacitance of the transparent grid layer of the ionic gel reduces the operating voltage. The corresponding voltage of the dirac point is positive, which indicates that the device is p-type.
Fig. 4a shows the output curves of an n-type photo-detection device at different gate voltages. As shown in fig. 4a, it indicates that the source-drain current and the source-drain voltage present a better linear relationship, and there is no saturation region, and graphene half-metallic property is still represented after doping. Meanwhile, the absolute value of the source-drain current increases with the increase of the absolute value of the gate voltage, which shows that the larger the gate voltage is, the more obvious the regulation and control of the carrier transmission of the device are. Fig. 4b shows the transfer curves of an n-type photo-detection device at different gate voltages. As shown in fig. 4b, the curve is approximately parabolic in shape, indicating that doping does not change the bipolar transmission characteristics of graphene; the corresponding voltage of the dirac point is negative, which indicates that the device is n-type.
Figure 5 shows the photodetector performance of the photodetecting device as a homogeneous semiconductor heterojunction. As shown in fig. 5, the heterojunction (i.e., the heterojunction formed by the n-type graphene and the p-type graphene) has a performance curve of the n-type graphene transistor in the n region and a performance curve of the p-type graphene transistor in the p region. And a depletion region is arranged between the n region and the p region and conforms to the curve required by the light detection device. That is, the light detection device can be prepared by the manufacturing method.
It should be noted that, although the flexible optical detection device based on graphene and the manufacturing method thereof are described above by taking the above embodiments as examples, those skilled in the art can understand that the disclosure should not be limited thereto. In fact, the user can flexibly set each step and part according to personal preference and/or actual application scene as long as the technical scheme of the disclosure is met.
Having described embodiments of the present disclosure, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terms used herein were chosen in order to best explain the principles of the embodiments, the practical application, or technical improvements to the techniques in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.

Claims (10)

1. A method for manufacturing a flexible graphene-based optical detection device, the method comprising:
etching a metal layer prepared in advance according to a preset shape to obtain an etched metal layer, wherein the etched metal layer is provided with a fixing part;
growing a first single-layer graphene on the etched metal layer fixed by the fixing part in a chemical vapor deposition mode;
after a temporary substrate layer is prepared on the first single-layer graphene, removing the etched metal layer;
transferring the first single-layer graphene with the temporary substrate layer to a first metal electrode on a pre-prepared flexible substrate, and removing the temporary substrate layer;
selectively doping the first single-layer graphene to obtain doped graphene;
placing pre-prepared undoped single-layer graphene on a second metal electrode on the flexible substrate, wherein a contact area exists between the undoped single-layer graphene and the doped graphene;
and preparing a transparent grid layer on the top of the device, wherein a part of region of the transparent grid layer covers the position, corresponding to the contact region, on the undoped single-layer graphene, so as to obtain the flexible light detection device.
2. The method of claim 1, wherein growing a first monolayer of graphene on the etched metal layer by chemical vapor deposition comprises:
after the etched metal layer is fixedly placed in a vacuum quartz tube by using the fixing part, pressurizing the quartz tube to a preset pressure, introducing hydrogen, heating to a first temperature, and keeping the first temperature for a first time;
continuously introducing hydrogen into the quartz tube at a first flow rate, and simultaneously introducing methane gas at a second flow rate, so that graphene grows on the etched metal layer;
and stopping introducing the methane gas after the duration of keeping the introducing states of the hydrogen gas and the methane gas reaches a second duration, so as to obtain the etched metal layer with the first single-layer graphene.
3. The method of claim 1, wherein selectively doping the first single-layer graphene to obtain a doped graphene comprises:
placing a bearing part with a protrusion on a region to be doped of the first single-layer graphene, wherein only the protrusion in the bearing part is in contact with the region to be doped of the first single-layer graphene, and a solution to be doped is coated on the protrusion;
and applying pressure to the bearing part to enable the solution to be doped to dope the first single-layer graphene so as to obtain doped graphene.
4. The method of claim 3, wherein the shape of the load bearing member comprises a pyramidal shape,
when the bearing part is in the pyramid shape, the top of the pyramid shape serves as the protrusion.
5. The method of claim 1, further comprising:
preparing an electrode metal layer on a flexible substrate;
etching the electrode metal layer to form a first metal electrode and a second metal electrode to obtain a flexible substrate with the first metal electrode and the second metal electrode,
wherein a space exists between the first metal electrode and the second metal electrode.
6. The method of claim 5, further comprising:
before selectively doping the first single-layer graphene, etching the first single-layer graphene, so that part of the etched first single-layer graphene covers the first metal electrode, and the other part of the etched first single-layer graphene is suspended among the intervals.
7. The method of claim 1, wherein removing the post-etch metal layer after preparing a temporary substrate layer on the first single-layer graphene comprises:
and removing the etched metal layer by using a removing liquid which only reacts with the etched metal layer.
8. The method of claim 1, wherein fabricating the transparent gate layer on top of the device comprises:
placing a liquid fence around the flexible substrate to form a bearing groove;
after the ionic gel liquid is added into the bearing groove, exposing the ionic gel liquid according to a preset pattern shape, so that polymerization reaction required for forming a transparent gate layer is generated at the exposed position in the ionic gel liquid;
and removing the unexposed ionic gel liquid on the flexible substrate to obtain the transparent gate layer.
9. The method of claim 5, further comprising:
and filling an insulating substance in the space between the first metal electrode and the second metal electrode.
10. A flexible graphene-based optical detection device, wherein the device is manufactured by the method of any one of claims 1-9, the device comprising: a flexible substrate (1), a first metal electrode (2), a second metal electrode (3), doped graphene (4), undoped single-layer graphene (5) and a transparent gate layer (6),
the first metal electrode (2) and the second metal electrode (3) are positioned on the flexible substrate (1), and a space exists between the first metal electrode (2) and the second metal electrode (3);
part of the doped graphene (5) is positioned on the first metal electrode (2), and the other part of the doped graphene is positioned between the intervals;
the undoped single-layer graphene (4) is positioned on the second metal electrode (3), and a contact area exists between the undoped single-layer graphene and the doped graphene (5);
the transparent gate layer (6) is positioned on the top of the device, and a partial area of the transparent gate layer (6) covers a position corresponding to the contact area on the undoped single-layer graphene (4).
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