CN114062457A - Vertical graphene electrochemical electrode detection chip and manufacturing method thereof - Google Patents
Vertical graphene electrochemical electrode detection chip and manufacturing method thereof Download PDFInfo
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- CN114062457A CN114062457A CN202111350525.4A CN202111350525A CN114062457A CN 114062457 A CN114062457 A CN 114062457A CN 202111350525 A CN202111350525 A CN 202111350525A CN 114062457 A CN114062457 A CN 114062457A
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- 238000001514 detection method Methods 0.000 title claims abstract description 41
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
Abstract
The invention discloses a vertical graphene electrochemical electrode detection chip and a manufacturing method thereof, wherein the vertical graphene electrochemical electrode detection chip comprises: the integrated detection chip comprises a substrate and a vertical graphene layer growing on the substrate, wherein one or more sets of grooves are prefabricated on the substrate, the vertical graphene layer grows and fills in the grooves, and one or more integrated detection chip structures of electrochemical electrodes are formed; the height of the vertical graphene layer is smaller than or equal to the depth of the groove. The manufacturing method comprises the following steps: providing a base material, and prefabricating one or more sets of grooves on the base material; growing a vertical graphene layer in the groove; and processing the vertically grown graphene layer to enable the upper surface of the vertically grown graphene layer to be flush with the upper surface of the substrate. The groove on the substrate has a protection effect on the fragile nano-scale vertical graphene layer, the thickness of the detection chip is reduced to a certain extent, and the stability and reliability of subsequent application are improved.
Description
Technical Field
The invention relates to the technical field of electrochemical electrode detection chip design, in particular to a vertical graphene electrochemical electrode detection chip and a manufacturing method thereof.
Background
The vertical graphene is a carbon artificial crystal nano material with a two-dimensional complex structure, has a large effective specific surface area, excellent conductivity and a large number of structural defects, is easy to modify various catalyst particles and chemical biomolecules, and is very suitable for being applied to materials for electrochemical and biochemical detection electrodes. The existing vertical graphene electrode is formed by depositing carbon atoms on a substrate through chemical vapor deposition on the substrate, so as to form a vertical graphene electrode protruding out of the surface of the substrate. However, the vertical graphene layer is macroscopic fragile, is afraid of scraping and wiping and cannot resist direct contact of foreign matters. The large surface area is also easy to be contaminated by various pollutants such as tiny dust, so that the active substance loses the effect, and the large-scale popularization and application of the active substance as an electrode in the industry are not facilitated.
Therefore, a brand new structure of the vertical graphene electrochemical test electrode chip is constructed to improve the stability of the vertical graphene electrochemical test electrode chip, improve the application scenario of the vertical graphene electrochemical test electrode chip, and broaden the application requirements of the vertical graphene electrochemical test electrode chip, which is a technical problem to be solved by those skilled in the art.
Disclosure of Invention
In order to solve the technical problems, the invention provides a vertical graphene electrochemical electrode detection chip and a manufacturing method thereof. The structure of the vertical graphene electrochemical electrode detection chip is optimally designed, so that the stability of the vertical graphene layer is greatly improved, and the technical scheme disclosed by the invention is as follows:
first, the present invention provides a vertical graphene electrochemical electrode detection chip, including: the detection device comprises a substrate and a vertical graphene layer grown on the substrate, wherein one or more sets of grooves are prefabricated on the substrate, and the vertical graphene layer is grown and filled in the grooves to form one or more electrochemical detection electrode structures; the height of the vertical graphene layer is smaller than or equal to the depth of the grooves, and the multiple sets of grooves have the same or different shapes.
Furthermore, the shape of each set of grooves is designed according to the design requirements of the electrochemical testing electrode.
Further, the grooves are formed by one or more of mechanical engraving, laser etching, radiation bombardment, or chemical reaction.
Further, the height of the vertical graphene layer is 1-50 μm.
Further, the base material is an insulating film, and the base material is one or more of PET, PE, PC, a thin glass sheet, a wafer silicon wafer, alumina ceramic and silicon nitride ceramic.
Furthermore, a through hole is formed in the base material, and a conductive substance is filled in the through hole; the back of the base material is provided with a plurality of pins and circuits, and the vertical graphene layer is electrically connected with the pins through the conductive substances in the through holes and the circuits.
Further, the conductive substance is a metal or a conductive carbon material.
Secondly, the invention also provides a manufacturing method of the vertical graphene electrochemical electrode detection chip, which comprises the following steps:
providing a base material, and prefabricating one or more sets of grooves on the base material;
growing a graphene material on the substrate;
and processing the substrate on which the vertical graphene material grows, and removing the graphene material grown outside the groove on the substrate, so that the upper surface of the vertical graphene layer grown in the groove is not higher than the upper surface of the substrate.
Further, the method of forming the groove includes: one or more of mechanical engraving, laser etching, radiation bombardment, or chemical reaction.
Further, the growth method of the vertical graphene layer is chemical vapor deposition.
Further, the method for processing the finished vertical graphene layer comprises the following steps: laser engraving, photoetching, machining, chemical etching and the like.
By adopting the scheme, the invention provides the vertical graphene electrochemical electrode detection chip and the manufacturing method thereof, and the vertical graphene electrochemical electrode detection chip has the following beneficial effects:
(1) through prefabricating the recess on the substrate, make the upright graphite alkene material that forms grow on the substrate in the recess, the upright graphite alkene electrochemistry electrode of making detects the upper surface of the layer of graphite alkene of standing vertically of chip and is not higher than the upper surface of substrate to this has realized the protection to upright graphite alkene layer, and it is more fragile to have solved the upright graphite alkene layer of graphite alkene electrochemistry electrode detection chip of standing vertically among the prior art, causes the condition of scraping damage easily, has improved the stability and the life of upright graphite alkene electrochemistry electrode detection chip greatly.
(2) The design is simple, the manufacture is convenient, and the batch production can be realized.
Drawings
FIG. 1 is a schematic diagram of a vertical graphene electrochemical electrode detection chip according to the present invention, in which a groove is preformed on a substrate.
Fig. 2 is a schematic diagram of a vertical graphene layer formed by the vertical graphene electrochemical electrode detection chip manufactured by the present invention after the vertical graphene layer is grown in the preformed groove.
Fig. 3 is a schematic structural diagram of a plurality of electrochemical electrodes arranged side by side on the vertical graphene electrochemical electrode detection chip of the present invention.
Detailed Description
The invention is described in detail below with reference to the figures and the specific embodiments.
As shown in fig. 1 to 3, the present invention provides a vertical graphene electrochemical electrode detection chip, including: a substrate 10 and a standing graphene layer 20 grown on the substrate 10. As shown in fig. 1, a groove 11 is prepared on the substrate 10, and the vertical graphene layer 20 is grown and filled in the groove 11 to form an electrochemical detection electrode structure. It is worth mentioning that the height of the vertical graphene layer 20 is less than or equal to the depth of the groove 11, that is, in the vertical graphene electrochemical electrode detection chip of the present invention, the surface of the vertical graphene layer 20 is lower than or flush with the surface of the substrate 10. This design has effectively protected upright graphite alkene layer 20, has solved the upright graphite alkene layer among the prior art and has outstanding in the substrate surface, and upright graphite alkene layer easily receives damage such as scraping, leads to electrode poor stability, is difficult to the problem of extensive application and popularization. And the thickness of the electrode is reduced to a certain extent, which is beneficial to the application of electrode miniaturization integration.
The number of the grooves 11 may be one or more, and correspondingly, the number of the formed electrochemical detection electrode structures is also one or more, as shown in the schematic diagram of fig. 3, a plurality of electrochemical detection electrode structures are arranged side by side on the vertical graphene electrochemical detection chip of the present invention. The shape of each set of grooves 11 is not limited, and is designed according to the circuit requirements of the electrochemical detection electrode, and in fig. 3, a plurality of sets of grooves have the same shape to form the same electrochemical detection electrode, while in other embodiments, a plurality of sets of grooves may also have different shapes according to the design requirements of the electrode to form different electrochemical detection electrodes. All fall within the scope of the present invention. The grooves 11 are formed by one or more of mechanical engraving, laser etching, radiation bombardment or chemical reaction.
In this embodiment, the substrate 10 is an insulating film, which may be one or more of PET, PE, PC, thin glass sheet, wafer silicon wafer, alumina ceramic, and silicon nitride ceramic.
In a preferred embodiment, the height of the grooves 11 and the upstanding graphene layer 20 is 1-50 μm.
The vertical graphene electrochemical electrode detection chip can be in a front-surface electric connection mode or a back-surface electric connection mode.
In a preferred embodiment (not shown), the substrate 10 is provided with a via hole filled with a conductive material such as a conductive metal or a conductive carbon material; the back of the substrate is provided with a plurality of pins and circuits, and the vertical graphene layer 20 is electrically connected with the pins through the conductive substance in the through holes and the circuits.
The invention also provides a manufacturing method of the vertical graphene electrochemical electrode detection chip, which comprises the following steps:
s10, providing a substrate 10, wherein the substrate 10 is an insulating film which can be PET, PE, PC thin glass sheet, wafer silicon sheet, alumina ceramic, silicon nitride ceramic, etc., and the thickness thereof is controlled to be 100 μm-10 mm. One or more sets of grooves 11 are prefabricated on the base material 10 through mechanical engraving, laser etching, radiation bombardment or chemical reaction, and the like, wherein the shape of each set of grooves 11 is designed according to the requirements of an electrochemical detection electrode circuit and is not limited.
S20, growing a vertical graphene material on the substrate 10, wherein the vertical graphene material is grown by a chemical vapor deposition method. Specifically, the cleaned and dried substrate 10 is placed in a PECVD apparatus, and vacuum is pumped to 10 deg.C-2To 100 Pa.
Introducing a carbon source gas and a formula gas, wherein the carbon source gas comprises: one or more of methane, ethane, propane, acetylene, propylene, the formulation gas comprising: one or more of nitrogen, argon, oxygen, hydrogen and air. And starting the PECVD equipment to perform plasma enhanced chemical vapor deposition to grow and form the vertical graphene layer 20, wherein the power of the PECVD equipment is set to be 200-2000w, the growth time of the vertical graphene layer is 5-100min, and the vertical graphene material is formed, and the thickness of the vertical graphene material is 1-50 mu m.
And S30, processing the substrate 10 with the vertical graphene materials grown, and removing the graphene materials grown outside the grooves on the substrate 10. The processing method comprises laser engraving, photoetching, machining, chemical etching and the like, so that the upper surface of the vertical graphene layer 20 grown in the groove is not higher than the upper surface of the substrate 10.
According to the vertical graphene electrochemical electrode detection chip, the groove in the substrate has a protection effect on the fragile vertical graphene layer, the manufacturing method is simple, and batch production can be realized. The vertical graphene layer is arranged in the groove, so that the thickness of the vertical graphene electrochemical electrode detection chip is reduced to a certain extent, the application of the vertical graphene electrochemical electrode detection chip in miniaturization integration is facilitated, and the vertical graphene electrochemical electrode detection chip is worthy of being widely popularized and used.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A vertical graphene electrochemical electrode detection chip is characterized by comprising: the detection device comprises a substrate and a vertical graphene layer grown on the substrate, wherein one or more sets of grooves are prefabricated on the substrate, and the vertical graphene layer is grown and filled in the grooves to form one or more electrochemical detection electrode structures; the height of the vertical graphene layer is smaller than or equal to the depth of the grooves, and the multiple sets of grooves have the same or different shapes.
2. The vertical graphene electrochemical electrode detection chip according to claim 1, wherein each set of grooves is designed according to electrochemical test electrode design requirements.
3. The vertical graphene electrochemical electrode detection chip according to claim 2, wherein the height of the vertical graphene layer is 1-50 μm.
4. The vertical graphene electrochemical electrode detection chip according to claim 1, wherein the substrate is an insulating thin film, and the substrate is one or more of PET, PE, PC, thin glass sheet, wafer silicon wafer, alumina ceramic, and silicon nitride ceramic.
5. The vertical graphene electrochemical electrode detection chip according to any one of claims 1 to 4, wherein a via hole is formed in the substrate, and a conductive material is filled in the via hole; the back of the base material is provided with a plurality of pins and circuits, and the vertical graphene layer is electrically connected with the pins through the conductive substances in the through holes and the circuits.
6. The vertical graphene electrochemical electrode detection chip according to claim 5, wherein the conductive material is a metal or a conductive carbon material.
7. The method for manufacturing the vertical graphene electrochemical electrode detection chip as claimed in any one of claims 1 to 6, comprising the following steps:
providing a base material, and prefabricating one or more sets of grooves on the base material;
growing a graphene material on the substrate;
and processing the substrate on which the vertical graphene material grows, and removing the graphene material grown outside the groove on the substrate, so that the upper surface of the vertical graphene layer grown in the groove is not higher than the upper surface of the substrate.
8. The method for manufacturing the vertical graphene electrochemical electrode detection chip according to claim 7, wherein the method for forming the groove comprises: one or more of mechanical engraving, laser etching, radiation bombardment, or chemical reaction.
9. The method for manufacturing the vertical graphene electrochemical electrode detection chip according to claim 7, wherein the vertical graphene layer is grown by chemical vapor deposition.
10. The method for manufacturing the vertical graphene electrochemical electrode detection chip according to claim 7, wherein the method for processing the vertical graphene layer after growth comprises: one or more of laser engraving, photolithography, machining, chemical etching.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111350525.4A CN114062457A (en) | 2021-11-15 | 2021-11-15 | Vertical graphene electrochemical electrode detection chip and manufacturing method thereof |
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| CN202111350525.4A CN114062457A (en) | 2021-11-15 | 2021-11-15 | Vertical graphene electrochemical electrode detection chip and manufacturing method thereof |
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| US20210147999A1 (en) * | 2019-11-19 | 2021-05-20 | University Of Central Florida Research Foundation, Inc. | Vertically-aligned graphene-carbon fiber hybrid electrodes and methods for making same |
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