CN117939999A - Flexible Hall sensing device based on graphene cross nano strips - Google Patents
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Abstract
The invention discloses a flexible Hall sensing device based on graphene cross nano strips, which is prepared by inducing silicon nanowires with uniform diameters to grow on a flexible substrate on which silicon dioxide is deposited; transferring the silicon nanowires on one flexible substrate sample to another flexible substrate sample with the silicon nanowires, and keeping the nanowires on the two flexible substrate samples mutually crossed and perpendicular; cleaning graphene with photoresist on a copper wire, and transferring the cleaned graphene to a flexible substrate deposited with a passivation layer; covering the prepared thin film with the crossed silicon nanowires on a flexible substrate covered with graphene, and defining a rectangular area to be etched to obtain an area to be prepared with crossed vertical graphene nano strips; and etching the graphene in the area which is not covered by the vertical crossing nanowire by taking the vertical crossing nanowire as a template, and obtaining the vertical crossing graphene nano strip in the covered area.
Description
Technical Field
The invention relates to preparation of a Hall sensing element, in particular to a method for etching a graphene cross nano strip Hall sensing prototype device by taking a planar growth silicon nanowire as a template, and a method for integrating the prepared graphene cross nano strip Hall sensing prototype device with a probe, belonging to the technical field of magnetic field detection and nano.
Background
The Hall sensor is the most important magnetic sensor, has the advantages of no contact, strong anti-interference capability and good linearity, and is widely applied to the fields of displacement sensing, current detection, mechanical detection and geomagnetic field detection. The basic principle is that a device with a current (I) in a magnetic field (B) will generate a transverse voltage (UH) perpendicular to the current direction. Therefore, the size of the magnetic field can be measured by testing the transverse voltage, the sensitivity is an important parameter for measuring the performance index of the Hall sensor, and the sensitivity characterizes the sensitivity degree of the sensor to magnetic field signals. The current sensitivity and the voltage sensitivity can be obtained by microscopic deduction: s_i=1/nqd, s_v=μw/L, where s_ I, S _v is current and voltage sensitivity, respectively, n is carrier concentration, q is unit charge quantity, d is hall device working substance thickness, μ is mobility, and W and L are device length and width, respectively. It is known that a high mobility, low carrier concentration, thin working material gives a hall detector with high sensitivity. Semiconductor materials have low carrier concentrations compared to metals, and are well suited for use in the fabrication of hall devices, silicon, germanium, and III-V semiconductor materials with high mobility are widely used for hall sensing, such as InSb, gaAs, and two-dimensional electron gas structures.
With the development of everything interconnection and wearable electronics, new requirements are put on integration and flexibility, and in particular, the magnetic imaging resolution of human beings in characterizing microstructures is higher and higher, so that smaller hall devices with higher integration are needed. Conventional hall devices are limited in process and have failed to meet the requirements due to severe performance degradation after device miniaturization.
Graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials, micro-nano processing, energy sources, biomedicine, drug delivery and the like, the carrier mobility of intrinsic suspended graphene at room temperature is about 200000 cm < 2 >/(V.s), and graphene with atomic layer thickness only has the unique advantage in Hall sensing, and meanwhile, even if the size is in the nanometer range, the mobility performance of graphene is still excellent, and the natural flexibility enables the graphene to be widely researched and applied in the aspect of wearable flexible electronics.
At present, some Hall sensing devices for preparing graphene cross nanoribbons also appear internationally, but the research team of the family discovers that the preparation of the prior art requires expensive electron beam etching, thereby greatly limiting the wide application of the preparation.
Therefore, the inventor provides a method for generating planar nanowires by metal induction based on lithography, the planar cross silicon nanowire array is formed by transfer assembly, and cross graphene nanoribbons are etched by taking the planar cross silicon nanowire array as a template.
Disclosure of Invention
The application solves the problem of high cost for preparing the graphene cross nanoribbons in the prior art by providing the flexible Hall sensor device based on the graphene cross nanoribbons, and realizes a method for preparing large-area and high-integration cross graphene nanoribbons and Hall sensors by adopting low cost.
The application provides a preparation method of a flexible Hall sensor device based on graphene cross nano strips, which is characterized by comprising the following steps:
1) Inducing the growth of silicon nanowires with uniform diameters on a flexible substrate on which silicon dioxide is deposited;
2) Transferring the silicon nanowires on one flexible substrate sample to another flexible substrate sample with the silicon nanowires, and keeping the nanowires on the two flexible substrate samples mutually crossed and perpendicular;
3) Cleaning the graphene with photoresist growing on the copper mesh, and transferring the cleaned graphene to a flexible substrate deposited with a passivation layer;
4) Covering the thin film with the crossed silicon nanowires prepared in the step 2) on the flexible substrate covered with the graphene in the step 3), defining a rectangular area to be etched, and developing and fixing to obtain an area to be prepared with crossed vertical graphene nano strips;
5) Etching the graphene in the area which is not covered by the vertical crossing nanowire by taking the vertical crossing nanowire as a template, and obtaining a vertical crossing graphene nano strip in the covered area;
6) Placing the flexible substrate upwards on the surface of an acetone solution to remove the silicon nanowire template;
7) The Hall electrode is prepared by photoetching and electron beam evaporation technology and is connected with an external circuit by a wire bonding packaging technology.
Preferably, the silicon nanowire in the step 1 is a nanowire with the surrounding amorphous silicon removed, the diameter of the nanowire is tens of nanometers to hundreds of nanometers, and the silicon nanowire is a single nanowire or an array.
Preferably, the transferring method of the silicon nanowire in the step2 is as follows:
Firstly, coating a photoresist layer on the surface of a sample with a silicon nanowire and drying;
Then, the sample is put in diluted hydrofluoric acid solution, and when photoresist floats in the solution, the film is fished out of the solution and dried;
Secondly, placing a photoresist film with the silicon nanowires on another silicon nanowire sample on a microscope transfer platform with angle scales, and enabling two layers of silicon nanowires to be vertical;
And finally, removing the photoresist film by using an acetone solution, drying the sample, spin-coating a layer of photoresist on the crossed nanowire sample, drying, placing the sample in a diluted hydrofluoric acid solution, and fishing out and drying the film when the film floats.
Preferably, the step of step 3 includes:
Firstly, spin-coating photoresist on graphene growing on a copper mesh, then placing the graphene into ammonium persulfate solution to corrode the copper mesh, transferring transparent graphene with photoresist into deionized water by using glass sheets after 2 hours, and cleaning for many times;
then, the graphene with the photoresist is transferred onto a substrate covered with a layer of silicon dioxide polyimide PI, and naturally dried in the shade without removing the photoresist.
Preferably, the thickness of the silicon dioxide in the step 3 is 90nm or 280 nm.
The invention also discloses a flexible Hall sensing device based on the graphene cross nano-strips, which is characterized in that: the device comprises a Hall detection element, an electrical channel and a CMOS readout circuit; the Hall detection element comprises a flexible substrate and two vertically crossed graphene nano strips or vertically crossed graphene nano strip arrays arranged on the flexible substrate;
The electrical channel is a Hall electrode arranged on the vertically crossed graphene nano strip or array and is used for switching on current and outputting Hall voltage;
the Hall electrode is a CMOS steady-flow input and readout circuit externally connected to the Hall electrode through a spot welding technology; the circuit includes a hall voltage amplifier and a signal processing circuit.
Preferably, the flexible substrate is a flexible polyimide PI substrate or polyethylene terephthalate PET.
Preferably, the passivation layer deposited on the flexible substrate is a flat silicon dioxide passivation layer, an aluminum oxide film, a hafnium oxide or a silicon nitride dielectric film.
The invention also discloses an application of the Hall device based on the graphene cross nano-strip, which is characterized in that the Hall detection element is adopted and fixed on the surface tip of the probe curvature radius tip by a pasting or bonding method, so as to measure a nano scanning probe of a microstructure or a biomedical nano molecular probe.
The technical scheme provided by the application has at least the following technical effects or advantages:
1) The invention adopts the cross silicon nanowire with the growth morphology programming, can prepare templates with any array and parameter, takes the templates as templates to etch and copy the graphene, and prepares the Hall device based on the etched graphene.
2) The flexible Hall device array can be prepared by selecting the substrate, and is applied to any curved surface, so that the flexible Hall device array meets the testing requirements of magnetic field, current, voltage and the like in special environments; the Hall nano probe can be prepared and applied to detection of a space high-resolution magnetic field, and the space distribution of the magnetic field can be obtained through scanning and is used for determining the space distribution condition of a magnetic material.
3) According to the invention, the planar growth silicon nanowire with the diameter of hundreds of nanometers to tens of nanometers is used as a template, the graphene cross nano strip can be obtained without expensive electron beam lithography technology, and meanwhile, the graphene has the advantages of high mobility, ultrathin thickness, high temperature stability and the like, so that the miniature high-integration high-sensitivity Hall sensing element can be obtained.
4) According to the invention, the flexible Hall sensor can be well attached to the surface with a large curvature radius by the natural flexibility and good mechanical characteristics of the graphene, and favorable conditions are provided for preparing the Hall sensing probe.
Drawings
Fig. 1 is a schematic view of a flexible nano hall device prepared in example 1 of the present invention.
Fig. 2 is a main flow chart of the preparation of the flexible nano hall device in embodiment 1 of the present invention.
FIG. 3 is a schematic view of a flexible nano Hall probe tip of the present invention.
Detailed Description
In order to better understand the above technical solutions, the following detailed description will refer to the accompanying drawings and specific embodiments.
Example 1
The embodiment provides a method for preparing a graphene nano strip Hall device by using a crisscrossed silicon nanowire as a template. As shown in fig. 1-2: the method comprises the following main steps:
1) A silicon nanowire is grown on a substrate with silicon dioxide using a Plasma Enhanced Chemical Vapor Deposition (PECVD) metal induced planar silicon nanowire growth technique (IPLSS), as shown in fig. 2 (a).
Preferably, the silicon nanowire sample mentioned in the step is a nanowire with the surrounding amorphous silicon removed, the diameter of the nanowire is uniform, the value of the nanowire can be tens of nanometers to hundreds of nanometers, the nanowire is thicker and better under the condition of no high integration level requirement according to the specific integration level requirement; the nanowires may be single nanowires or arrays, and the embodiment is described in detail by taking nanowire arrays as an example.
2) The silicon nanowires on one sample are transferred to another sample with silicon nanowires and the two sample nanowires are kept perpendicular to each other. Specifically, a photoresist layer is coated on the surface of a sample with nanowires and dried, then the sample is placed in a diluted hydrofluoric acid solution, and when the photoresist floats in the solution, the film is fished out of the solution and dried; placing a photoresist film with silicon nanowires on another silicon nanowire sample on a microscope transfer platform with angle scales, and enabling two layers of silicon nanowires to be vertical;
As a preferred embodiment, the method of transferring the silicon nanowire and assembling the nanowire under a microscope by using an optical fiber probe is shown in fig. 2 (b);
3) Removing the photoresist film by using an acetone solution, drying the sample, spin-coating a photoresist layer on the cross silicon nanowire sample, drying, placing the sample in a diluted hydrofluoric acid solution, and fishing out and drying the film when the film floats.
4) And (2) after spin coating photoresist on the graphene growing on the copper mesh, placing the graphene into ammonium persulfate solution to corrode the copper mesh, transferring transparent graphene with photoresist into deionized water by using a glass sheet after 2 hours, cleaning for many times, and then transferring the graphene with photoresist onto a silicon dioxide Polyimide (PI) substrate covered with a layer, and naturally drying in the shade without removing the photoresist, as shown in fig. 2 (c).
Preferably, the thickness of the silicon dioxide in this example is chosen to be 90nm. The inventor researches find that the graphene can be found and the thickness of the graphene can be judged through the color when the thickness of the silicon dioxide is 90nm or 280 nm, and other thicknesses can also be used, but the graphene can not be found and the thickness of the graphene can not be judged quickly and conveniently.
5) Covering the thin film with the crossed silicon nanowires prepared in the step 3 on the PI substrate with the graphene prepared in the step 4, defining a rectangular area to be etched by a photoetching method, developing and fixing, and thus obtaining the area to be prepared with the crossed graphene nano strips.
6) Etching off the graphene at the unmasked position by using the cross silicon nanowire as a template and using a Reactive Ion Etching (RIE) technology, so that a cross graphene nano strip is obtained at the area masked by the nanowire, as shown in fig. 2 (d);
7) Placing a sample PI substrate upwards on the surface of an acetone solution, and removing a silicon nanowire template;
8) The hall electrode was prepared by photolithography and electron beam evaporation techniques and connected to an external circuit by wire bonding techniques, as shown in fig. 2 (e). Preferably, the hall electrode in this embodiment may be titanium/gold, or may be another metal electrode such as tungsten, aluminum, copper, or the like.
Preferably, the photoresist used in the above steps may be a photoresist such as SU8 or AZ 5214.
In the graphene cross structure of the embodiment, graphene provides a material with high mobility, and the cross structure can increase the width W and reduce the length L, so that high voltage sensitivity is provided.
Example 2
This example provides a method of preparing a graphene nanoribbon hall probe based on example 1. The flexible Hall sensing probe provided by the embodiment comprises a Hall detection element, an electrical channel, a CMOS reading circuit and an element surface passivation structure.
The hall detection element in the embodiment is a vertically crossed graphene nano strip array; the electrical channel is a Hall electrode arranged on the vertically crossed graphene nano strip array and is used for switching on current and outputting Hall voltage; the Hall electrode is a CMOS steady-flow input and readout circuit externally connected to the Hall electrode through a spot welding technology; the circuit comprises a Hall voltage amplifier and a signal processing circuit.
The embodiment also comprises a passivation structure with a passivation layer deposited on the surface of the element, and the passivation layer is covered with a flexible substrate of the Hall detection element.
In this embodiment, the hall device and the substrate are fixed on the tip of the probe by means of adhesion or bonding, and then connected with an external circuit by means of bonding, and the effect is shown in fig. 3. A nano scanning probe or biomedical nano molecular probe for measuring microstructure.
Preferably, the flexible substrate of the present embodiment is a flexible polyimide PI substrate, or polyethylene terephthalate PET.
Preferably, the passivation layer deposited on the flexible substrate in this embodiment is a flat silicon dioxide passivation layer, an aluminum oxide film, a hafnium oxide or a silicon nitride dielectric film.
The foregoing is merely a preferred embodiment of the invention, and it should be noted that modifications could be made by those skilled in the art without departing from the principles of the invention, which modifications would also be considered to be within the scope of the invention.
Claims (9)
1. The preparation method of the flexible Hall sensor device based on the graphene cross nano strips is characterized by comprising the following steps of:
1) Inducing the growth of silicon nanowires with uniform diameters on a flexible substrate on which silicon dioxide is deposited;
2) Transferring the silicon nanowires on one flexible substrate sample to another flexible substrate sample with the silicon nanowires, and keeping the nanowires on the two flexible substrate samples mutually crossed and perpendicular;
3) Cleaning the graphene with photoresist growing on the copper mesh, and transferring the cleaned graphene to a flexible substrate deposited with a passivation layer;
4) Covering the thin film with the crossed silicon nanowires prepared in the step 2) on the flexible substrate covered with the graphene in the step 3), defining a rectangular area to be etched, and developing and fixing to obtain an area to be prepared with crossed vertical graphene nano strips;
5) Etching the graphene in the area which is not covered by the vertical crossing nanowire by taking the vertical crossing nanowire as a template, and obtaining a vertical crossing graphene nano strip in the covered area;
6) Placing the flexible substrate on the surface of an acetone solution to remove the silicon nanowire template;
7) The Hall electrode is prepared by photoetching and electron beam evaporation technology and is connected with an external circuit by a wire bonding packaging technology.
2. The method for manufacturing the flexible hall sensor device based on the graphene cross nano-strips, which is disclosed in claim 1, is characterized in that the silicon nanowire in the step 1 is a nanowire with surrounding amorphous silicon removed, the diameter of the nanowire is tens of nanometers to hundreds of nanometers, and the silicon nanowire is a single nanowire or an array.
3. The method for preparing the flexible hall sensor device based on the graphene cross nano-strips according to claim 1, wherein the transferring method of the silicon nanowires in the step 2 is as follows:
Firstly, coating a photoresist layer on the surface of a sample with a silicon nanowire and drying;
Then, the sample is put in diluted hydrofluoric acid solution, and when photoresist floats in the solution, the film is fished out of the solution and dried;
Secondly, placing a photoresist film with the silicon nanowires on another silicon nanowire sample on a microscope transfer platform with angle scales, and enabling two layers of silicon nanowires to be vertical;
And finally, removing the photoresist film by using an acetone solution, drying the sample, spin-coating a layer of photoresist on the crossed nanowire sample, drying, placing the sample in a diluted hydrofluoric acid solution, and fishing out and drying the film when the film floats.
4. The method for manufacturing a flexible hall sensor device based on graphene cross nano-strips according to claim 1, wherein the step of step 3 comprises:
Firstly, spin-coating photoresist on graphene growing on a copper mesh, then placing the graphene into ammonium persulfate solution to corrode the copper mesh, transferring transparent graphene with photoresist into deionized water by using glass sheets after 2 hours, and cleaning for many times;
then, the graphene with the photoresist is transferred onto a substrate covered with a layer of silicon dioxide polyimide PI, and naturally dried in the shade without removing the photoresist.
5. The method for manufacturing a flexible hall sensor device based on graphene cross nano-strips according to claim 1, wherein the thickness of silicon dioxide in the step3 is 90nm or 280 nm.
6. A flexible hall sensing device based on graphene cross nano strips is characterized in that: the device comprises a Hall detection element, an electrical channel and a CMOS readout circuit; the Hall detection element comprises a flexible substrate and two vertically crossed graphene nano strips or vertically crossed graphene nano strip arrays arranged on the flexible substrate;
The electrical channel is a Hall electrode arranged on the vertically crossed graphene nano strip or array and is used for switching on current and outputting Hall voltage;
the Hall electrode is a CMOS steady-flow input and readout circuit externally connected to the Hall electrode through a spot welding technology; the circuit includes a hall voltage amplifier and a signal processing circuit.
7. The graphene-cross-nanoribbon-based flexible hall sensing device according to claim 6, wherein: the flexible substrate is a flexible polyimide PI substrate or polyethylene terephthalate PET.
8. The graphene-cross-nanoribbon-based flexible hall sensing device according to claim 6, wherein: the passivation layer deposited on the flexible substrate is a flat silicon dioxide passivation layer, an aluminum oxide film, hafnium oxide or silicon nitride dielectric film.
9. An application of a Hall sensing device based on graphene cross nano-strips is characterized in that the Hall sensing element is adopted, and the Hall sensing element is fixed on the surface of a probe curvature radius needle point by a pasting or bonding method and is used for measuring a microstructure nano scanning probe or a biomedical nano molecular probe.
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| CN202410108528.4A CN117939999A (en) | 2024-01-25 | 2024-01-25 | Flexible Hall sensing device based on graphene cross nano strips |
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| CN202410108528.4A CN117939999A (en) | 2024-01-25 | 2024-01-25 | Flexible Hall sensing device based on graphene cross nano strips |
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