WO2021240640A1 - Électrode en film mince de carbone et son procédé de fabrication - Google Patents

Électrode en film mince de carbone et son procédé de fabrication Download PDF

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Publication number
WO2021240640A1
WO2021240640A1 PCT/JP2020/020724 JP2020020724W WO2021240640A1 WO 2021240640 A1 WO2021240640 A1 WO 2021240640A1 JP 2020020724 W JP2020020724 W JP 2020020724W WO 2021240640 A1 WO2021240640 A1 WO 2021240640A1
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film
electrode
multilayer graphene
thin film
self
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PCT/JP2020/020724
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English (en)
Japanese (ja)
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東一郎 後藤
哲彦 手島
真澄 山口
祐子 上野
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日本電信電話株式会社
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Priority to PCT/JP2020/020724 priority Critical patent/WO2021240640A1/fr
Priority to JP2022527313A priority patent/JP7343822B2/ja
Publication of WO2021240640A1 publication Critical patent/WO2021240640A1/fr

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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

Definitions

  • the present invention relates to a carbon thin film electrode and a method for manufacturing the same.
  • the single-layer graphene has a conical band structure and can be used as a channel of an electrochemical FET (Field Effect Transistor).
  • an electrochemical FET Field Effect Transistor
  • the detection target can be detected with high sensitivity as a change in drain current due to charge redistribution on the channel surface (Non-Patent Document 1). ..
  • Graphene has a wider potential window than gold, which is a typical electrode material, and does not easily oxidize in solution like silicon and gallium.
  • the edge of graphene has high chemical reaction activity due to the presence of dangling bonds (a type of unpaired electron). Due to these characteristics, research and development using single-layer graphene as a working electrode for electrochemical measurement and a non-metal electrode for hydrogen generation is also being carried out (Non-Patent Document 2). Further, single-layer graphene has high light transmittance and is expected as a transparent electrode.
  • Non-Patent Document 3 discloses an example in which CVD-grown multilayer graphene is used as a channel for a spintronics device.
  • Multi-layer graphene does not have high light transmission like single-layer graphene, but it is stronger than single-layer graphene and has a small effect on conductivity when impurities adhere to the surface.
  • multi-layer graphene has higher conductivity than single-layer graphene due to its multi-layer structure, has abundant edge dangling bonds, and has higher reactivity than single-layer graphene, so it can be applied to high-precision electrochemical sensors. You can expect it.
  • HOPG Highly Oriented Pyrolytic Graphite
  • the carbon thin film obtained by ECR (Electron Cyclotron Resonance) sputtering is a kind of multilayer graphene in which a graphene layer is vertically formed on a part of the surface of a base substrate.
  • the detection accuracy is lowered because there are few dangling bonds that can be effectively reacted with the detected substance.
  • the graphene surface (basal surface) also participates in the reaction depending on the detected substance.
  • graphene grown by CVD is generally flat with respect to the surface of the substrate, and one side of the graphene is in close contact with the substrate, so that it cannot contribute to the reaction. Therefore, there is also a problem that one side of graphene grown by CVD cannot be effectively used as an electrode or a channel.
  • the present invention has been made in view of the above circumstances, and includes a multilayer graphene in which the graphene surface can efficiently contribute to the reaction with the detection substance and has many dangling bonds capable of reacting with the detection substance. It is an object of the present invention to provide a carbon thin film electrode and a method for producing the same.
  • the present invention employs the following means.
  • the carbon thin film electrode according to one aspect of the present invention is made of a multilayer graphene film in which a plurality of graphene films are laminated and a material formed on one main surface of the multilayer graphene film and having a younger rate than that of the multilayer graphene film. Due to the gradient of the internal stress in the thickness direction due to the difference in the Youngness ratio between the multilayer graphene film and the material having a Younger ratio smaller than that of the multilayer Graphene membrane in the direction orthogonal to the thickness direction.
  • the three-dimensional structure has a self-forming portion that self-forms, and is formed on an electrode formed on one main surface of the graphene film and on the other main surface of the graphene film in a portion excluding the self-forming portion. Further prepare for the sacrificial membrane that has been made.
  • the method for manufacturing a carbon thin film electrode according to one aspect of the present invention is the method for manufacturing a carbon thin film electrode according to any one of (1) to (6) above, wherein a sacrificial film is formed on one main surface of the substrate.
  • the multilayer graphene film is self-formed in the three-dimensional structure, the dangling bond at the edge of the multilayer graphene film is separated from the substrate surface and easily comes into contact with the detection substance. It has become. Further, since the graphene surface is separated from the substrate surface and exposed to the reaction environment, the reactivity of the graphene surface is also enhanced. Therefore, in the carbon thin film electrode of the present invention, the multilayer graphene film is in a state of having many dangling bonds and graphene surfaces capable of reacting with the detection substance, and when applied as a multilayer graphene electrode, its reactivity is enhanced. Can be done.
  • FIG. 1 It is a perspective view of the carbon thin film electrode which concerns on 1st Embodiment of this invention.
  • A It is a top view of the self-forming part which constitutes a carbon thin film electrode.
  • B Of the self-forming portions of (a), it is an enlarged view of the portion surrounded by a broken line.
  • A), (b) It is sectional drawing of the object to be processed in the manufacturing process of a carbon thin film electrode.
  • (A)-(c) is a cross-sectional view and a plan view of an object to be processed in the process of manufacturing a carbon thin film electrode.
  • A), (b) is a cross-sectional view, plan view of the object to be processed in the manufacturing process of a carbon thin film electrode.
  • (A), (b) It is a perspective view of the object to be processed in the manufacturing process of a carbon thin film electrode. It is a perspective view of the object to be processed in the manufacturing process of a carbon thin film electrode. It is a figure which shows typically the structure of the electrochemical sensor which applied the carbon thin film electrode. It is a photograph of the self-forming part of the carbon thin film electrode which concerns on (a) and (b) Examples 1 and 2. It is a graph which shows the electric property of the carbon thin film electrode obtained by the carbon thin film electrode of Example 2.
  • FIG. 1 is a perspective view of a carbon thin film electrode 100 according to an embodiment of the present invention.
  • the carbon thin film electrode 100 mainly includes a multilayer graphene film 104, a stress adjusting film 105, an electrode 106, and a sacrificial film 107.
  • the carbon thin film electrode 100 includes a self-forming unit 101 that self-forms a state in which the multilayer graphene film 104 is warped (a state of three-dimensional structure), and an electrode installation unit 102 that installs an electrode 106 that connects to an external power source. The case where the self-forming portion 101 and the electrode installation portion 102 are connected to each other is illustrated.
  • the self-forming portion 101 and the electrode portion B may be directly connected without passing through the connecting portion 103, but in that case, the self-forming portion is easily distorted and the self-forming portion 101 may be damaged. It is preferable to use the portion 103.
  • the width of the connecting portion 103 is preferably about 1/10 to 1/5 of the width of the self-forming portion 101.
  • the multilayer graphene film 104 is formed by laminating a plurality of graphene films.
  • multilayer graphene films There are various types of multilayer graphene, but those grown by CVD on a metal film are preferable in consideration of film quality such as flatness and uniformity of the number of layers.
  • the number of laminated graphene films constituting the multilayer graphene is preferably 10 to 300.
  • Nickel is often used for CVD growth of multilayer graphene because it is easy to control the number of layers. If the number of layers is more than 300, the flexibility is lowered and the warp is less likely to occur, which hinders self-formation into the three-dimensional structure described later. On the contrary, when the number of layers is less than 10, the surface area of the edge portion becomes small, so that the dangling bonds are reduced and the durability of graphene is also lowered.
  • the stress adjusting film 105 is formed on one main surface 104a of the multilayer graphene film, and is made of a material having a Young's modulus smaller than that of the multilayer graphene film 104.
  • the Young's modulus of the stress adjusting film 105 is preferably in the range of 1 to 20% of the Young's modulus of the multilayer graphene film 104.
  • the stress adjusting film 105 may be a dielectric material that can be formed on the multilayer graphene film 104, is easier to evaluate electrical characteristics than metals and semiconductors, and is electrically and chemically inert. Is preferable.
  • the stress adjusting film 105 has a thickness (0.1 to 0) that bends freely when an internal stress gradient is formed in the thickness direction 104d of the two films due to the difference in Young's modulus from the multilayer graphene film 104. It has about 5.5 ⁇ m).
  • parylene has a Young's modulus of 2.4 GPa (when the film thickness is 0.6 ⁇ m) and the multilayer graphene obtained by CVD growth is 15 to 30 GPa, so that an internal stress gradient is likely to occur in the thickness direction, and the three-dimensional structure has a three-dimensional structure. Since it is advantageous for self-formation, it is particularly preferable as a material for the stress adjusting film 105.
  • FIG. 2A is a plan view of the self-forming portion 101 of the carbon thin film electrode.
  • the self-forming portion 101 the state in which the multilayer graphene film 104 is warped (curved) due to the gradient of internal stress in the direction orthogonal to the thickness direction 104d due to the difference in Young's modulus between the stress adjusting film 105 and the multilayer graphene film 104 is self. It is formed.
  • the multilayer graphene 104 and the stress adjusting film 105 in the self-forming portion 101 are both warped so as to form a part of the side wall surface of the virtual cylinder, but are located at one end 101a and the other end 101b of the self-forming portion in the expansion / contraction direction.
  • the edges 104c of the multilayer graphene need to be separated from each other.
  • the self-forming portion 101 may be multiple-wound (overlapping) around the central axis of the virtual cylinder.
  • FIG. 2 (b) is an enlarged view of the self-forming portion 101 of FIG. 2 (a) surrounded by a broken line.
  • FIGS. 2A and 2B when a part of the self-forming portion on the one end 101a side and a part on the other end 101b side overlap with each other in the thickness direction 104d of the multilayer graphene film 104, both are used.
  • the edges 104c of the multilayer graphene film do not come into direct contact with each other even if they are in contact with each other. Therefore, the dangling bonds 108 of both edges 104c of the multilayer graphene film do not bond with each other and are exposed on the surface.
  • both edges 104c of the multilayer graphene film can be separated from the substrate. This makes it easier for the detection substance to come into contact with the edge 104c of the multilayer graphene, and it is possible to prevent the contact of the detection substance from being hindered by the depositary substance on the substrate. Furthermore, the warping of the multilayer graphene 101 also exposes the dangling bonds formed on the surface other than the edge 104c, so that more detection substances can be brought into contact with each other.
  • the graphene surface does not come into contact with the surface of the substrate, it is exposed to an environment that easily reacts with the detected substance, so that the graphene area is doubled and the reactivity is improved. As a result, the reactivity of the carbon thin film electrode 100 with respect to the detected substance can be enhanced.
  • the electrode 106 is formed on one main surface 104a of the graphene film in the portion (electrode mounting portion 102) excluding the self-forming portion 101.
  • the material of the electrode 106 is not particularly limited as long as it has conductivity. Generally, metals suitable for vapor deposition and sputtering such as platinum, gold, chromium, titanium, nickel, copper and aluminum are used.
  • the sacrificial film 107 is formed on the other main surface 104b of the graphene film in the portions (electrode mounting portion 102 and connection portion 103) excluding the self-forming portion 101.
  • the sacrificial film 107 has a Young's modulus of about 0.5 MPa to 3 MPa in the case of gel and a Young's modulus of about 50 GPa to 300 GPa in the case of metal, and suppresses warping like the multilayer graphene film 101 of the self-forming portion 101. Has a function.
  • the sacrificial film 107 cannot be easily peeled off without peeling work, and the film thickness of the sacrificial film 107 is 3 nm or more when the sacrificial film 107 is a metal and 50 nm or more when the sacrificial film 107 is a gel. It is preferable to have.
  • the material of the sacrificial film 107 may be any material that can be peeled off (removed) from the adhered multilayer graphene film 104 without damaging the multilayer graphene film 104, and examples thereof include metals such as aluminum and copper. .. If it is aluminum or iron, it is preferable as a material for the sacrificial membrane 107 because it can be removed by the sacrificial membrane alone by immersing it in a sodium hydroxide aqueous solution (concentration 1 M) or MicropositTM 351 Developer for about 1 to 5 minutes. Copper can be quickly removed by immersing it in a solution in which equal amounts of aqueous ammonia (3M) and aqueous hydrogen peroxide (3 to 30%) are mixed.
  • aqueous ammonia 3M
  • aqueous hydrogen peroxide 3 to 30%
  • copper is immersed in an aqueous solution of sodium glutamate (1 to 5 g / 20 mL), 1 to 5 g of sodium chloride and 4 to 10 mL of hydrogen peroxide solution (3 to 30%), or an aqueous solution of iron (III) chloride.
  • sodium glutamate (1 to 5 g / 20 mL
  • sodium chloride 1 to 5 g of sodium chloride
  • hydrogen peroxide solution 3 to 30%
  • iron (III) chloride an aqueous solution of iron (III) chloride
  • the thickness of the sacrificial film 107 is about 10 to 200 nm.
  • the metal sacrificial film can be formed by performing sputtering, EB vapor deposition, or the like.
  • Aqueous sodium alginate solution (1% wt) is filtered through a hydrophilic filter (200 nm pore diameter), spin coated on a solid substrate (2000 to 4000 rpm, about 30 seconds), and then put into a calcium chloride aqueous solution (0.1 M) for 10 seconds.
  • a thin film that has been immersed and gelled may be used as a sacrificial film.
  • the sacrificial membrane can be peeled off by adding EDTA (5 mM).
  • the carbon thin film electrode 100 can be manufactured mainly through the following steps.
  • a plurality of graphene films 101 are laminated on the metal film 109 to form a multilayer graphene film.
  • the metal used for CVD growth of multilayer graphene include copper, chromium, and nickel.
  • Nickel is suitable for CVD growth of multilayer graphene having a well-organized number of layers because nickel can easily control the number of layers.
  • the metal film 109 is peeled (removed) from the multilayer graphene film 101 using a stripping solution or the like (multilayer graphene film forming step).
  • the nickel film thickness is preferably 50 to 200 ⁇ m.
  • the timing of removal is not specified, if the multilayer graphene from which the metal film has been peeled off is transferred to the substrate and then removed, there is no effect on the subsequent process.
  • the protective film can be removed with an organic solvent such as acetone without damaging the sacrificial layer or graphene.
  • one main surface 110a of the substrate 110 is cleaned by performing piranha or oxygen plasma treatment, and then a known film forming method such as a sputtering method, an EB vapor deposition method, or a spin coating method is selected. Then, as shown in FIG. 4A, the sacrificial film 107 is formed (sacrificial film forming step).
  • the material of the substrate 110 may be, for example, glass, silicon, plastic, or the like, which is flat and can be used in a normal semiconductor process.
  • the multilayer graphene film 104 obtained through the multilayer graphene film forming step is mounted (transferred) on the sacrificial film 107 that has undergone the sacrificial film forming step (mounting the multilayer graphene film). Process).
  • the electrode 106 is placed at a predetermined position on the multilayer graphene film 104 as shown in FIG. 4 (c) (cross-sectional view on the top and plan view on the bottom).
  • Form electrode forming step
  • a stress adjusting film 105 made of a material having a Young's modulus smaller than that of the multilayer graphene film 104 is formed. , Formed on the outermost surface after electrode formation (stress adjustment film forming step).
  • the region to be the self-forming portion 101 and the connecting portion 103 is covered with the mask 111, and the stress adjusting film 105 in the region not covered by the mask 111 is covered with the oxygen plasma P. Is irradiated and etched. As a result, as shown in FIG. 6A, the stress adjusting film 105 is formed only on the self-forming portion 101 and the connecting portion 103.
  • the mask 111 a metal mask or a resin mask produced by a 3D printer may be used, or patterning by photolithography or electron beam lithography may be combined with etching by oxygen plasma or UV ozone.
  • the sacrificial membrane removing liquid L such as EDTA is dropped only on the portion of the sacrificial membrane 107 contained in the self-forming portion 101, and the sacrificial membrane 107 is dissolved and removed (sacrificed). Membrane removal step).
  • the self-forming portion 101 is surrounded by the side wall of the well-shaped (cylindrical) container 112, and the sacrificial membrane removing liquid L is dropped only into the container 112 to form an electrode. It is possible to prevent the sacrificial film 107 of the installation portion 102 and the connection portion 103 from being accidentally removed.
  • the multilayer graphene film 104 is self-formed in a warped state due to the gradient of the internal stress due to the difference in Young's modulus between the stress adjusting film 105 and the multilayer graphene film 104.
  • the carbon thin film electrode 100 can be obtained as shown in FIG.
  • the sacrificial film removing liquid L is dropped on the entire sample in the sacrificial film removing step. However, the entire pattern is not removed. Therefore, the container 112 becomes unnecessary.
  • the multilayer graphene film 104 is self-formed in the three-dimensional structure, the dangling bond 108 at the edge 104c of the multilayer graphene film is formed on the surface of the substrate 110. It is far from the area and is in a state where it can easily come into contact with the detected substance. Therefore, in the carbon thin film electrode 100 of the present embodiment, the multilayer graphene film 104 is in a state of having many dangling bonds 108 capable of reacting with the detection substance, and when applied as a working electrode or a channel of an electrochemical FET, The reactivity can be enhanced.
  • the carbon thin film electrode 100 of the present embodiment is manufactured by transferring and microfabricating the multilayer graphene film 104 on the substrate, the sensor structure for electrochemical measurement can be turned on-chip.
  • the carbon thin film electrode 100 of the present embodiment can be used as an FET channel or an electrode for hydrogen generation in addition to the working electrode for electrochemical measurement.
  • FIG. 8 is a diagram schematically showing a configuration example of an electrochemical sensor 10 in which a carbon thin film electrode 100 is turned on-chip.
  • the electrochemical sensor 10 mainly determines the potentials of the working electrode 11, the counter electrode 12, the reference electrode 13, the electrolytic solution 14 in which the three electrodes are immersed, the reaction layer 15 containing the electrolytic solution 14, and the three electrodes.
  • the counter electrode 12 has a larger surface area than the working electrode.
  • edge 104c of the multilayer graphene film 104 of the self-forming portion 101 is patterned in an uneven shape, more dangling bonds 108 can be formed. Further, even in the case of a three-dimensional structure other than the cylindrical shape, a highly accurate working electrode can be obtained if the structure has a large number of dangling bonds 108.
  • the carbon thin film electrode of the above embodiment was manufactured by the following procedure.
  • the glass substrate was treated with oxygen plasma (100 W, oxygen partial pressure 30 Pa) for 10 minutes, and 1% -sodium alginate was added dropwise to the substrate for spin coating (3000 rpm, 30 seconds).
  • the glass substrate on which the sacrificial film made of sodium alginate was formed was immersed in a CaCl 2 aqueous solution for about 60 minutes to gel the sodium alginate.
  • the concentration of the CaCl 2 aqueous solution was about 100 mM. After the immersion, the glass substrate on which the sacrificial film was formed was thoroughly washed with water to remove water.
  • a multilayer graphene film formed by laminating 60 layers of graphene film was formed on a nickel thin film.
  • the nickel thin film was peeled off from the formed multilayer graphene film and transferred onto the substrate on which the sacrificial film was formed.
  • An electrode was formed on the multilayer graphene film, and then a parylene thin film having a thickness of 120 nm was formed by a vapor deposition method. Oxygen plasma etching was performed after covering the self-forming part and the connecting part with a mask. Finally, 1-5 mM EDTA was dropped onto the sacrificial membranes of the self-forming part and the connecting part, and these were removed to obtain a carbon thin film electrode.
  • Example 2 A carbon thin film electrode was obtained by evaporating 200 mg of a parylene thin film and setting the thickness to 125 nm under the same conditions as in Example 1.
  • FIG. 9 (a) and 9 (b) are photographs and schematic cross-sectional views of the carbon thin film electrodes obtained in Examples 1 and 2, respectively.
  • the self-forming portion before self-forming is a square of 100 ⁇ m square.
  • a substantially cylindrical three-dimensional structure as shown in FIG. 2 is self-formed, the ends having dangling bonds overlap each other in the thickness direction, and one of them penetrates inside the other.
  • Example 2 since the parylene film was formed thickly, the self-formed three-dimensional structure had a small warp and the ends did not overlap each other. From these results, it can be seen that the shape of the three-dimensional structure of the self-forming portion can be controlled by adjusting the thickness of the stress adjusting film.
  • FIG. 10 is a graph showing the electrical characteristics obtained by the carbon thin film electrode of Example 2. It can be seen that the linear current-voltage characteristics are obtained and the current value is sufficient as a working electrode.
  • Example 2 an average of 60 layers of multi-layer graphene was used, but if the number of layers is within the range in which self-formation is possible, the conductivity can be increased by increasing the number of layers.
  • a conductive molecule having high biocompatibility for example, PEDOT: PSS, can be modified on the surface of the multilayer graphene by a known electrochemical method. This makes it possible to obtain a working electrode having a high affinity with biological substances such as proteins and biological tissues while maintaining conductivity.

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Abstract

La présente invention concerne une électrode en film mince de carbone (100) comprenant : un film de graphène multicouche (104) dans lequel une pluralité de films de graphène sont stratifiés ; et un film de réglage de contrainte (105) formé sur une surface principale (104a) du film de graphène multicouche et constitué d'un matériau présentant un module de Young inférieur à celui du film de graphène multicouche (104), une partie auto-formante (101) se formant automatiquement en une structure tridimensionnelle en fonction du gradient dans l'épaisseur de contrainte interne dû à la différence de module de Young dans une direction perpendiculaire à la direction de l'épaisseur (104d) entre le film de graphène multicouche (104) et le matériau (105) présentant un module de Young inférieur à celui du film de graphène multicouche. Dans une partie excluant la partie auto-formante (101), l'électrode en film mince de carbone comprend en outre : une électrode (106) formée sur une surface principale (104a) du film de graphène ; et un film sacrificiel (107) formé sur l'autre surface principale (104b) du film de graphène.
PCT/JP2020/020724 2020-05-26 2020-05-26 Électrode en film mince de carbone et son procédé de fabrication WO2021240640A1 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
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WO2023157691A1 (fr) * 2022-02-17 2023-08-24 東京エレクトロン株式会社 Procédé de traitement de substrat et appareil de traitement de substrat

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WO2014208184A1 (fr) 2013-06-28 2014-12-31 株式会社 日立ハイテクノロジーズ Dispositif d'analyse
US10381107B2 (en) 2016-12-05 2019-08-13 Government Of The United States Of America, As Represented By The Secretary Of Commerce Nucleic acid sequencer for electrically determining a sequence of nitrogenous bases in a single stranded nucleic acid

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JP2020008358A (ja) * 2018-07-04 2020-01-16 日本電信電話株式会社 微小電極、及びその製造方法、並びに集積デバイス

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
WO2023157691A1 (fr) * 2022-02-17 2023-08-24 東京エレクトロン株式会社 Procédé de traitement de substrat et appareil de traitement de substrat

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