WO2017119715A1 - Dispositif et procédé d'inspection de graphène - Google Patents

Dispositif et procédé d'inspection de graphène Download PDF

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Publication number
WO2017119715A1
WO2017119715A1 PCT/KR2017/000095 KR2017000095W WO2017119715A1 WO 2017119715 A1 WO2017119715 A1 WO 2017119715A1 KR 2017000095 W KR2017000095 W KR 2017000095W WO 2017119715 A1 WO2017119715 A1 WO 2017119715A1
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Prior art keywords
graphene film
liquid
graphene
image information
image
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PCT/KR2017/000095
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English (en)
Korean (ko)
Inventor
주상현
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경기대학교 산학협력단
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Publication of WO2017119715A1 publication Critical patent/WO2017119715A1/fr

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B3/00—Drying solid materials or objects by processes involving the application of heat
    • F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
    • F26B3/06—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air the gas or vapour flowing through the materials or objects to be dried
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
    • G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/08—Measuring arrangements characterised by the use of optical techniques for measuring diameters
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/26—Measuring arrangements characterised by the use of optical techniques for measuring angles or tapers; for testing the alignment of axes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02—Investigating surface tension of liquids
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/95—Investigating the presence of flaws or contamination characterised by the material or shape of the object to be examined
    • G—PHYSICS
    • G06—COMPUTING; CALCULATING OR COUNTING
    • G06T—IMAGE DATA PROCESSING OR GENERATION, IN GENERAL
    • G06T7/00—Image analysis

Definitions

  • the present invention relates to an apparatus and an inspection method for inspecting the properties of graphene.
  • Graphene is a two-dimensional structure made of carbon and has advantages of high mobility and conductivity, as well as transparency and flexibility. These characteristics of graphene can overcome the limitations of device implementations that occur in conventional displays, semiconductor devices, sensors, supercapacitors, and solar cells. For example, by replacing the existing transparent electrode (ITO electrode or IZO electrode) with graphene having a transparent and bendable characteristics, it is possible to manufacture various types of transparent electrodes as well as lower the manufacturing cost.
  • ITO electrode or IZO electrode transparent and bendable characteristics
  • graphene In order for graphene to be applied to an actual commercially available device, it is important to grow well so that there are almost no defects.
  • Graphene is generally formed on a surface of a metal, such as copper or nickel, and then transferred from the metal surface to an insulating substrate.
  • Graphene grows with defects such as vacancies, interstitial atoms, non-carbon atoms, and lattice reconstruction.
  • graphene is grown after tearing or stretching due to physical impact during transfer, transfer and removal of poly (methyl methacrylate) (PMMA), annealing, and cleaning with acetone. Couplings such as doping by PMMA occur.
  • PMMA poly (methyl methacrylate)
  • Raman spectroscopy is one of the most widely used analytical methods for examining the characteristics of graphene such as the presence of defects.
  • X-ray photoelectron spectroscopy, transmission electron microscopy, scanning tunneling microscope, atomic force microscopy In addition, there are analysis methods using Auger electron spectroscopy and laser photo analysis.
  • Existing analytical methods are capable of accurate and diverse analysis of graphene characteristics, but it takes a long time to obtain analytical results, and requires expensive equipment.
  • existing analytical methods do not directly analyze the graphene film grown on the surface of the metal substrate, thus transferring the grown graphene to another insulator substrate or mesh grid. The process is necessary. Therefore, the existing analytical methods have a problem that it is not possible to determine whether the defects found in the analysis of graphene occurred in the process of growing graphene or in the process of transferring graphene.
  • An object of the present invention is to provide an inspection apparatus and an inspection method capable of inspecting the characteristics of graphene in real time without transferring the graphene.
  • the graphene inspection device of the present invention is a device for inspecting the characteristics of the graphene film including whether the graphene film is defective, the injection nozzle unit for forming a liquid droplet by spraying a liquid on the upper surface of the graphene film; At least one of a diameter, a height, and a contact angle of the graphene film from the image information generating unit and the image information generating unit for generating image information of the shape of the liquid droplet formed on the graphene film; It characterized in that it comprises an image analyzer for determining whether a defect is generated in the graphene film by calculating a value.
  • the injection nozzle unit includes at least one injection nozzle for injecting the liquid on the upper surface of the graphene film, the injection nozzle is one on the upper surface of the graphene film by injecting the liquid of 0.01 ⁇ 200 ⁇ l each It can form the liquid drop of.
  • the liquid may be water or alcohol.
  • the image information generating unit may photograph the liquid droplets from the upper portion of the liquid droplets to generate first image information including information about the diameter of the liquid droplets, and the front and rear portions of the liquid droplets. And a second photographing unit configured to photograph the liquid drop from the side to generate second image information including information about a contact angle and a height of the liquid droplet of the graphene film.
  • the first photographing unit includes a first camera for photographing the first image information and a first transmission module for transmitting the first image information to the image analyzing unit, and the second photographing unit includes the second image information.
  • a second transmission module configured to transmit a second camera to photograph and the second image information to the image analyzer.
  • the first photographing unit or the second photographing unit may have the liquid droplet formed on the graphene film. The first image information or the second image information may be photographed after a shooting time interval of 0 to 30 seconds has elapsed.
  • first photographing unit or the second photographing unit may be formed to photograph one time or at least two times according to the photographing time interval.
  • the image analyzer may include at least one of a reference diameter, a reference height, and a reference contact angle calculated by forming the droplets on the graphene film without defects, and the diameter of the droplets is larger than the reference diameter. In this case, it may be determined that a defect is generated in the graphene film when the height of the liquid drop is lower than the reference height or when the contact angle of the liquid drop is smaller than the reference contact angle.
  • the image analyzer may generate alarm information when it is determined that a defect is generated in the graphene film, and may further include an alarm unit configured to receive the alarm information transmitted from the image analyzer and generate an alarm signal. have.
  • the graphene inspection apparatus may further include an image information display unit displaying first image information and second image information transmitted from the image analyzer.
  • the graphene inspection device may further include a droplet removing unit for removing the liquid droplets by supplying wind, hot air or light to the liquid droplets after the generation of the image information in the image generating unit.
  • the graphene inspection method of the present invention is a method for examining the characteristics of the graphene film including whether the graphene film is defective, liquid injection to form a liquid droplet by spraying a liquid on the upper surface of the graphene film And generating image information of the shape of the liquid drop formed on the top surface of the graphene film, and at least a diameter, a height of the liquid drop, and a contact angle with the graphene film from the image information. And calculating an image to determine whether a defect is generated in the graphene film.
  • the image analysis step using the at least one of the reference diameter, reference height and reference contact angle calculated by forming the liquid droplets on the graphene film without defects, the diameter of the liquid droplets than the reference diameter it may be determined that a defect is generated in the graphene film when the height of the liquid drop is lower than the reference height or when the contact angle of the liquid drop is smaller than the reference contact angle.
  • the liquid spraying step may inject a liquid of 0.01 ⁇ 200 ⁇ m on the upper surface of the graphene film at one time, it may proceed to form one of the liquid droplets in one spray.
  • the liquid spraying step may be made to spray a liquid at a position spaced apart from the upper surface of the graphene film in the width direction at the same time, a plurality of the liquid droplets are formed in the width direction of the graphene film.
  • the liquid may be water or alcohol.
  • the image information may include first image information including information about a diameter of the liquid droplet by photographing the liquid droplet from an upper portion of the liquid droplet, and photographing the liquid droplet from the front rear or side of the liquid droplet.
  • the image information may include second image information including information about a height of a liquid drop and a contact angle with respect to the graphene film.
  • the generating of the image information may be performed such that the first image information or the second image information is photographed after the liquid droplet is formed on the graphene film and a shooting time interval of 0 to 30 seconds has elapsed.
  • the first image information or the second image information may be made to photograph once or at least twice according to the photographing time interval.
  • the graphene inspection method generates alarm information when it is determined that a defect is generated in the graphene film in the image analysis step, and generates an alarm signal according to the alarm information after the image analysis step. It may further comprise a generating step.
  • the graphene inspection method may further include a drop removing step of removing the liquid drop by supplying hot air or irradiating light to the liquid drop after the image information generating step.
  • Graphene inspection apparatus and method according to the present invention has the effect that can be inspected in real time without transferring the graphene film on the characteristics including whether or not a defect is present in the graphene film grown on the metal substrate.
  • the graphene inspection apparatus and method according to the present invention excludes defects that may occur in the process of transferring the graphene from the metal substrate and examines only the defects generated in the growth process, the roll-to-roll method by the chemical vapor deposition method It is effective to accurately identify and replace in real time whether or not a problem occurs in the large-scale graphene growth process that is grown.
  • the graphene inspection apparatus and method according to the present invention has the effect of reducing the analysis time and analysis cost compared to the existing method without using expensive equipment (Raman spectroscopy or transmission electron microscope, etc.).
  • the graphene inspection apparatus and method according to the present invention removes the liquid sprayed on the upper surface of the graphene film for the inspection to use the graphene film as a normal production product when there is no defect in the graphene film There is an effect of minimizing the consumption of the graphene film according to the inspection.
  • FIG. 1 is a block diagram of a graphene inspection device according to an embodiment of the present invention.
  • FIG. 2 is a process chart of the graphene test method according to an embodiment of the present invention.
  • FIG. 3 is a schematic diagram of a liquid ejecting step, an image information generating step, and an image analyzing step in the process diagram of FIG. 2.
  • FIG. 4 is a graph showing a contact angle measurement result according to a defect of a graphene film grown on a metal substrate.
  • FIG. 5 is a graph showing a contact angle measurement result according to a defect after transferring a graphene film grown on a metal substrate to an insulating substrate.
  • FIG. 6 is a graph showing a measurement result of Raman characteristics according to a defect of a graphene film grown on a metal substrate.
  • FIG. 7 is a graph showing measurement results of Raman characteristics according to defects in graphene films after transferring graphene films grown on metal substrates to insulating substrates.
  • FIG. 10 is a graph showing a result of measuring the height of water droplets according to a defect of a graphene film grown on a metal substrate.
  • FIG. 11 is a graph illustrating a diameter measurement result of water droplets according to a defect of a graphene film grown on a metal substrate.
  • FIG. 1 is a block diagram of a graphene inspection device according to an embodiment of the present invention.
  • a graphene inspection apparatus includes a spray nozzle unit 110, an image information generator 120, and an image analyzer 130.
  • the graphene test apparatus may further include an image information display unit 140, an alarm unit 150, and a drop removing unit 160.
  • the graphene inspection apparatus sprays a liquid onto the surface of the graphene film (b) to form a liquid droplet (c) and the diameter, height of the liquid droplet (c) or the contact angle with the graphene film (b)
  • the shape is measured to evaluate the characteristics including whether the graphene film (b) is defective.
  • the spray nozzle unit 110 may include at least one spray nozzle 111 and may include a plurality of spray nozzles 111.
  • the spray nozzle unit 110 may be formed such that the plurality of spray nozzles 111 are spaced apart from each other in a line along the width direction of the graphene film b.
  • the spray nozzle unit 110 may include the spray nozzles 111 in a number corresponding to the number of inspection points in which the graphene film b is appropriately set along the width direction.
  • the injection nozzles 111 are spaced apart from each other according to the inspection interval required for the inspection in the width direction of the graphene film (b). Accordingly, the spray nozzle unit 110 includes a relatively large number of spray nozzles 111 when the graphene film b has a wide width, and the narrower the inspection interval, the relatively large number of spray nozzles 111. ) May be included.
  • the spray nozzle 111 sprays a liquid such as water or alcohol onto the surface of the graphene film b to form a liquid drop c.
  • the liquid may be a polymer solution or an organic solvent solution.
  • the liquid may be Dimethyl sulfoxide (DMSO), Chlorobenzene, Methanol, Toluene, Isopropanol, Acetone, Ethanol, oil, benzene, THF (L (-)-5,6,7,8-tetrahydrofolic acid), DMF ( dimethylformamide), Hexane, glycerol, cyclohexane, gasoline, diesel.
  • DMSO Dimethyl sulfoxide
  • Chlorobenzene Chlorobenzene
  • Methanol Toluene
  • Isopropanol Acetone
  • Ethanol oil
  • benzene THF (L (-)-5,6,7,8-tetrahydrofolic acid)
  • DMF dimethylformamide
  • the spray nozzle 111 is dropped onto the graphene surface in the form of a drop rather than spraying the liquid to be sprayed at a time in a mist state.
  • the injection nozzle 111 may be sprayed so that the liquid falls to the upper surface of the graphene film (b) by the free fall to form a liquid drop (c).
  • the liquid sprayed from the spray nozzle 111 forms a liquid drop c having the same or similar size on the surface of the graphene film b in the same state.
  • the injection nozzle 111 is formed to supply a predetermined amount of liquid.
  • the spray nozzle 111 may spray a liquid of 0.01 ⁇ 200 ⁇ l at a time.
  • the spray nozzle 111 may spray 0.1-50 ⁇ l of liquid at a time. More preferably, the injection nozzle 111 may inject 1 to 20 ⁇ l of liquid at a time.
  • the amount of the liquid sprayed by the spray nozzle 111 is too small, the size of the liquid drop c may be too small to make it difficult to measure the shape of the liquid drop c.
  • the amount of the liquid sprayed by the spray nozzle 111 is too large, it may be difficult for the liquid drop (c) to reflect the surface characteristics of the graphene film (b).
  • the injection nozzle unit 110 is a nozzle for moving the injection nozzle 111 in the width direction of the graphene film (b) when the number of the injection nozzle 111 is less than one or the number of inspection points required It may further comprise a moving means (115).
  • the nozzle moving means 115 continuously conveys the spray nozzle 111 at predetermined intervals in the width direction of the graphene film b. Therefore, the injection nozzle unit 110 forms a predetermined number of liquid droplets c in the width direction on the top surface of the graphene film b.
  • the nozzle moving means 115 may move the injection nozzle 111 in the width direction of graphene, such as a means including a motor and a ball screw, a means including a motor and a chain or a belt, and a means including an air cylinder. Which can be formed by various means.
  • the image information generating unit 120 generates image information of the liquid drop (c) formed on the upper surface of the graphene film (b).
  • the image information generating unit 120 may include a first photographing unit 121 and a second photographing unit 125.
  • the first photographing unit 121 and / or the second photographing unit 125 captures an image once after the liquid droplet c is formed on the graphene film b and a shooting time interval of 0 to 30 seconds has elapsed. You can do that.
  • the photographing time interval is set in consideration of the time required for the liquid droplet (c) to maintain a stable shape in the graphene film (b).
  • the liquid droplet (c) may take time from 0 seconds to several tens of seconds to stabilize while reacting with the surface of the graphene film (b) according to the type of liquid. That is, the liquid used in the liquid drop (c) can be stabilized immediately upon being seated on the graphene film (b).
  • the photographing time interval of 0 seconds means that immediately after the liquid droplet (c) is formed on the graphene film (b).
  • the liquid used in the liquid drop (c) may require a few seconds to be seated on the graphene film (b).
  • the shooting time interval is too short, the image may be taken before the liquid drop c is stabilized.
  • the shooting time interval is too long, the size of the liquid drop (c) may be reduced by evaporation of the liquid, depending on the type of liquid.
  • the shooting time interval may be longer than 30 seconds.
  • the diameter, height and contact angle of the liquid drop (c) may be measured. This is because the liquid droplet c stabilizes while reacting with the surface of the graphene film b, depending on the type of liquid and the type of substrate, which takes time from 0 to several tens of seconds. For example, the image capturing time intervals are set to 1 second and 5 seconds, respectively, and then the images may be compared and analyzed.
  • the first photographing unit 121 is formed to include a first camera 122 for photographing an image or a photo to generate first image information.
  • the first photographing unit 121 may further include a first transmitting module 123 that transmits the photographed first image information to the image analyzing unit 130.
  • the first photographing unit 121 is positioned in front of the spray nozzle unit 110 based on the flow direction of the graphene film b.
  • the first photographing unit 121 photographs the liquid droplet c from the upper portion of the liquid droplet c formed on the upper surface of the graphene film b grown on the metal substrate a. That is, the first photographing unit 121 photographs the liquid drop c from the upper portion of the vertical direction of the liquid drop c to generate first image information corresponding to the top view of the liquid drop c.
  • the first photographing unit 121 generates first image information when the liquid drop c formed by the liquid ejected from the spray nozzle unit 110 is transferred to the lower portion of the first camera 122.
  • the first photographing unit 121 is different due to the influence of the brightness or color of the liquid drop c based on the image information of the upper surface of the graphene film b in which the liquid drop c is not formed.
  • it may be determined that there is a liquid drop c and generate first image information.
  • the first camera 122 is formed to have a resolution that can clearly distinguish the boundary line of the liquid drop (c) formed on the surface of the graphene film (b).
  • the first camera 122 is formed in one or a plurality of images so as to capture all the liquid droplets (c) formed spaced apart in the width direction on the upper surface of the graphene film (b).
  • the first camera 122 is spaced apart a predetermined distance from the upper portion of the graphene film (b) to be continuously transported, the liquid droplet is formed in the upper surface of the graphene film (b) is injected from the injection nozzle 111
  • the first image information is generated by taking an image or a picture of c).
  • the first camera 122 preferably generates the first image information when the liquid drop c formed on the top surface of the graphene film b is located under the camera. Therefore, since the first camera 122 photographs the liquid drop c from the vertical upper portion of the liquid drop c, the first camera 122 always generates first image information on the liquid drop c constantly. Since the first image information is image information obtained by capturing the liquid drop c from the top, the first image information includes an image of the liquid drop c photographed in a circular shape.
  • the first transmission module 123 is connected to the first camera 122 and transmits the captured first image information to the analyzer.
  • the first transmission module 123 may be formed in various configurations used to transmit image information.
  • the second photographing unit 125 is formed to include a second camera 126 that photographs an image or a photo to generate second image information.
  • the second photographing unit 125 may further include a second transmitting module 127 which transmits photographed second image information to the image analyzing unit 130.
  • the second photographing unit 125 is positioned in front, rear, or side of the first photographing unit 121 based on the flow direction of the graphene film b.
  • the second photographing unit 125 may be linked with the first photographing unit 121 and may generate second image information simultaneously or after a set time according to a photographing signal transmitted from the first photographing unit 121.
  • the second photographing unit 125 may generate second image information when the liquid drop c is recognized from the front regardless of the first photographing unit 121.
  • the second photographing unit 125 photographs the liquid droplet c from the front, rear or side of the liquid droplet c formed on the upper surface of the graphene film b grown on the metal substrate a. That is, the second photographing unit 125 photographs the vertical shape of the liquid drop c to generate second image information corresponding to the front view, the rear view, or the side view of the liquid drop c.
  • the second camera 126 is formed to have a resolution that can clearly distinguish the boundary line of the liquid droplet (c) formed on the surface of the graphene film (b).
  • the second camera 126 is formed on one or a plurality of the plurality of liquid droplets (c) formed to be spaced apart in the width direction on the upper surface of the graphene film (b).
  • the second camera 126 is positioned at the same height as the upper surface of the graphene film (b) continuously transferred, the liquid droplet (c) is sprayed from the injection nozzle 111 formed on the upper surface of the graphene film (b)
  • the second image information is generated by taking an image or a picture of the front, rear or side of the camera.
  • the second camera 126 preferably generates the second image information in the vertical shape of the liquid drop c formed on the top surface of the graphene film b. Since the second image information is image information obtained by photographing the liquid drop c from the front, the second image information includes an image photographed in a circular, semi-circular, or arc shape.
  • the second transmission module 127 is connected to the second camera 126 and transmits the photographed second image information to the image analyzer 130.
  • the second transmission module 127 may be formed in various configurations used to transmit image information.
  • the second photographing unit 125 is omitted.
  • the first imaging unit 121 may be omitted.
  • the image analyzer 130 is interlocked with the image information generator 120 and the diameter, height, and graphene film (b) of the liquid droplet (c) from the image information transmitted from the image information generator 120. At least one value of the contact angle is calculated, and it is determined whether the reference angle with respect to the predetermined reference diameter, reference height or the graphene film (b) is out of the range. In this case, the image analyzer 130 determines whether at least one of the diameter, the height, and the contact angle of the liquid drop c deviates from the reference diameter, the reference height, and the reference contact angle, two values deviate, or three values. It may be determined that the defects are generated in the graphene film (b) by determining whether all the deviations.
  • the image analyzing unit 130 is connected to the first photographing unit 121 and the second photographing unit 125, and the first image information transmitted from the first photographing unit 121 and the second photographing unit 125.
  • the second image information transmitted is analyzed.
  • the image analyzer 130 includes at least one piece of information among a preset reference diameter, a reference height, and a reference contact angle with the graphene film b.
  • the reference diameter, reference height, and reference contact angle may vary depending on the type of liquid used, the amount of liquid sprayed, and the characteristics of the graphene film (b). Therefore, the reference diameter, reference height and the reference contact angle with the graphene film (b) is stored in advance for each graphene film (b) manufacturing line to which the graphene inspection device according to an embodiment of the present invention is applied It is necessary to do
  • the image analyzer 130 may transmit information about a time at which the first image information and the second image information are photographed to the first photographing unit 121 and the second photographing unit 125, respectively.
  • the first photographing unit 121 captures an image of the upper portion of the liquid drop c at the time when the liquid drop c is positioned below the first camera 122 to capture the first image information.
  • the second photographing unit 125 captures an image of the front surface of the liquid drop c at a time when the liquid drop c is located in front of the first camera 122 to generate second image information. can do.
  • the image analyzer 130 calculates a diameter having a size viewed from an upper surface of the liquid drop c from the first image information. In this case, the image analyzer 130 separates the liquid drop c from the periphery of the liquid drop c in the first image information to determine a planar shape of the liquid drop c and to determine the size of the liquid drop c. Measure In this case, the image of the liquid drop (c) is circular as described above.
  • the image analyzer 130 calculates the contact angle of the graphene film (b) of the liquid drop (c) and the height from the upper surface of the graphene film (b) from the second image information.
  • the image analyzer 130 separates the liquid drop c from the liquid drop c surrounding the liquid drop c in the second image information to determine the vertical shape of the liquid drop c, and the liquid drop c and the graphene film ( The contact angle of b) and the height from the upper surface of the graphene film (b) of the liquid drop (c) are calculated.
  • the image analyzer 130 may use a method of extracting the shape of the liquid drop c based on the brightness or the color of the liquid drop c from the first image information or the second image information. In addition, the image analyzer 130 may use various known methods for separating a specific shape from an image.
  • the image analyzer 130 may measure a diameter, a height, or a contact angle of a liquid drop (c) currently measured based on a reference diameter, a reference height, and a reference contact angle of a previously set liquid drop (c). It is determined in real time whether it is lower, and alarm information can be generated if necessary. That is, the image analyzer 130 may measure the diameter, height, and contact angle of the liquid droplet c currently being measured based on a reference diameter, a reference height, and a reference value of the reference contact angle of the liquid droplet c previously set. It may be determined in real time whether it is lower than the reference value. Therefore, the image analyzer 130 may determine in real time whether there is an abnormality in the graphene growth process currently being performed, and in the case of abnormality in the process, generate alarm information to identify the process stop and cause in real time. To proceed.
  • the image information display unit 140 includes an image display module capable of displaying an image, and displays the first image information and the second image information transmitted from the image analyzer 130.
  • the image information display unit 140 may display the diameter, height, or contact angle of the liquid drop c calculated from the first image information and the second image information.
  • the image information display unit 140 may be integrally formed with the image analyzer 130.
  • the alarm unit 150 includes a device such as a speaker or a warning lamp, and is connected to the image analyzer 130.
  • the alarm unit 150 receives alarm information from the image analyzer 130 and generates an alarm signal such as sound or light.
  • the alarm unit 150 may be integrally formed with the image analyzer 130.
  • the drop removing unit 160 is formed to include a means for supplying wind, hot air, heat or light.
  • the drop removing unit 160 is positioned in front of the second photographing unit 125 based on the flow direction of the graphene film b.
  • the drop removing unit 160 removes the liquid drop (c) formed on the upper surface of the graphene film (b) by supplying wind, hot air, heat or light to the upper surface of the graphene film (b). That is, the drop removing unit 160 removes the liquid drop c by supplying wind, hot air, heat, or light to the liquid drop c after the generation of the image information is completed by the image generating unit 120. Therefore, the liquid is not present on the upper surface of the graphene film (b) is completed by the graphene inspection device.
  • FIG. 2 is a process chart of the graphene test method according to an embodiment of the present invention.
  • 3 is a schematic diagram of a liquid ejecting step, an image information generating step, and an image analyzing step in the process diagram of FIG. 2.
  • 4 is a graph showing a contact angle measurement result according to a defect of a graphene film grown on a metal substrate.
  • 5 is a graph showing a contact angle measurement result according to a defect after transferring a graphene film grown on a metal substrate to an insulating substrate.
  • 6 is a graph showing a measurement result of Raman characteristics according to a defect of a graphene film grown on a metal substrate.
  • FIG. 7 is a graph showing measurement results of Raman characteristics according to defects in graphene films after transferring graphene films grown on metal substrates to insulating substrates.
  • 8 is a graph showing the correlation between the contact angle of the graphene film and Raman characteristics (I D / I G ).
  • 9 is a graph showing the correlation between the contact angle of the graphene film and Raman properties (I 2D / I G ).
  • 10 is a graph showing a result of measuring the height of water droplets according to a defect of a graphene film grown on a metal substrate.
  • FIG. 11 is a graph illustrating a diameter measurement result of water droplets according to a defect of a graphene film grown on a metal substrate.
  • FIG. It is a graph which shows the measurement result of the diameter of the water droplet with the defect of the graphene film grown on the metal base material.
  • the graphene inspection method includes a liquid injection step S20, an image information generation step S30, and an image analysis step S40.
  • the graphene test method may further include a reference value setting step S10, an alarm signal generating step S50, and a drop removing step S60.
  • the graphene film (b) to which the graphene inspection method is applied is grown and formed by the source material supplied to the surface of the metal substrate (a).
  • the metal substrate (a) is Ni, Co, Fe, Pt, Au, Al, Cr, Cu, Mg, Mn, Mo, Rh, Si, Ta, Ti, W, U, V, Zr, brass, bronze, white It may be formed of one or more metals or alloys selected from the group consisting of brass, stainless steel and Ge.
  • the metal substrate (a) may be further formed with a catalyst layer on the surface for the smooth growth of the graphene film (b).
  • the graphene inspection method according to the present invention may be applied even after the graphene film b is transferred to another substrate.
  • the substrate may be formed of corning glass, quartz, dielectric, or plastic substrate.
  • the graphene inspection method according to the present invention includes a flat panel display module, a semiconductor device, a solar cell module, and the like. It can also be applied to evaluate the properties of the graphene film used in the module in the various modules used and manufactured.
  • the graphene film (b) may be grown using any of a variety of growth methods, including chemical vapor deposition method commonly used for graphene growth in the art, for example, thermal vapor deposition process, Rapid Thermal Chemical Vapor Deposition (RTCVD) Process, Inductively Coupled Plasma-Chemical Vapor Deposition (ICP-CVD) Process, Low Pressure Chemical Vapor Deposition (LPCVD) Process, Atmospheric Pressure Chemical Vapor Deposition (APCVD) Process, Metal Organic Chemical Vapor Deposition (MOCVD) Process Plasma-enhanced chemical vapor deposition (PECVD) processes may be used, but are not limited now.
  • chemical vapor deposition method commonly used for graphene growth in the art, for example, thermal vapor deposition process, Rapid Thermal Chemical Vapor Deposition (RTCVD) Process, Inductively Coupled Plasma-Chemical Vapor Deposition (ICP-CVD) Process, Low Pressure Chemical Vapor Deposition (LPCVD) Process, Atmospheric Pressure Chemical Va
  • the reference value setting step (S10) is a step of setting a reference value for determining whether a defect exists in the graphene film (b).
  • the graphene film (b) may include defects due to various factors while growing on the surface of the metal substrate (a).
  • the graphene film (b) has a hydrophilicity (hydrophilicity) or hydrophobicity (hydrophobicity) characteristics change when it contains a defect therein.
  • hydrophilicity hydrophilicity
  • hydrophobicity hydroophobicity
  • the reference value setting step (S10) is set to the reference value by measuring the diameter, height, or contact angle of the water droplets formed by spraying water on the graphene film (b) is not generated defects. That is, the diameter, height, and contact angle of the water droplets formed by spraying water on the graphene film b in which the defect is not generated are set as the reference diameter, the reference height, and the reference contact angle, respectively.
  • the contact angle, height, and diameter of the water droplets formed on the upper surface of the graphene film (b) may be relatively changed according to the amount of water sprayed. Therefore, the amount of water sprayed on the graphene film (b) is set to be constant, the same as the amount of water sprayed in the actual graphene film (b) growth process.
  • the water may be sprayed in the range of 0.01 to 200 ⁇ l.
  • the water is not sprayed by the mist, it is sprayed at a low pressure to form water droplets on the upper surface of the graphene film (b).
  • the water may be sprayed to fall to the upper surface of the graphene film (b) by the free fall to form water droplets.
  • the graphene film may generate various kinds of defects in the growth process, and the ratio of defects generated may also vary.
  • the graphene film is a surface characteristic changes according to the type of defects and the ratio of defects generated. Therefore, the graphene film prepared with various defects was prepared and evaluated.
  • the graphene film has most defects of the defect-free graphene film (type 1), hydroxyl (hydroxyl) group and most of the defects of the graphene film (type 2), hydroxyl group (hydroxyl) of 2% or more defects 5% or more of the graphene film (type 3), carbonyl group (carbonyl) and ether (ether) and carboxyl group of the defects are most of the graphene film (type 4), the defect is more than 3%, Most of the defects of carbonyl and carboxyl groups were prepared, and graphene films (type 5, type 6, and type 7) having 7% or more of defects were prepared.
  • the liquid to be sprayed on the graphene film was made of water, and the amount of sprayed at once was 5 ⁇ l and five water droplets were formed for each type.
  • the contact angle and height and diameter of the water droplets to be measured below can be measured differently when using a different liquid, and the reference value can be set differently.
  • the contact angle with respect to the water droplet formed by spraying water while the graphene film is on a metal substrate was measured.
  • the contact angle of the type 1 was measured as 80.1 ⁇ 1.26 °
  • the contact angle is the highest in the graphene film without a bond, it can be seen that gradually decreases according to the ratio and type of defects.
  • the graphene film maintains hydrophobicity when there are no defects, so that the contact angle is the highest, and when the defects are generated, the contact angle has hydrophilicity and the contact angle decreases.
  • the result of measuring the contact angle with respect to each after transferring the graphene film same as the above to the insulating substrate is shown in FIG. Referring to FIG. 5, although the change in the absolute value of the measured contact angle is different for each type, it can be seen that the trend of the contact value is maintained as it is.
  • the reference value for the reference contact angle for determining whether or not the defect of the graphene film may be set to 70 °, preferably 75 °, more preferably 80 °. From the above results, the contact angle is measured in real time in the process of growing the graphene film in a roll-to-roll manner to determine whether a defect is generated in the graphene film when the contact angle is lower than the reference contact angle. In addition, the type and amount of defects generated in the graphene film may be evaluated from the contact angle of the graphene film.
  • I D / I G represents the intensity ratio of D Raman peak (1344 cm -1 ) and G Raman peak (1596 cm -1 )
  • I 2D / I G represents 2D Raman peak (2682 cm -1 ) and G Raman peak 6 shows the intensity ratio of and the frequency of defects generated in the graphene film.
  • FIG. 6 in the state where the graphene film is on a metal substrate, each type of graphene film shows the same Raman characteristics, and thus defect analysis through Raman characteristics was not possible.
  • the Raman characteristics are different for each type. Can be.
  • the graphene substrate without defects is relatively strong in the G peak and the 2D peak, while the intensity of the D peak is weak.
  • the intensity of the G peak and the 2D peak is relatively weak, while the intensity of the D peak is strong.
  • the graphene film compared the contact angle and Raman characteristics for each type. 8 and 9, the contact angle of each type of the graphene film has a constant correlation with the Raman property, and it can be seen that the physical properties of the graphene film including the presence of defects are shown. That is, when a defect is generated in the graphene film, the contact angle may be lowered and I D / I G may be increased.
  • the water droplets formed on the upper surface of the graphene film are lowered in height compared to the graphene film without defects, and are shown in the same manner as the change in contact angle.
  • the reference height for the height may be set to 1.4 to 1.5 mm. Therefore, when the height of the water droplets formed on the upper surface of the graphene film is lower than 1.4 ⁇ 1.5mm it can be determined that a defect is generated in the graphene film.
  • the height of the water droplets may vary slightly depending on the amount of water to be sprayed, it is necessary to determine a reference value according to the amount of water.
  • the change in the diameter of the water droplet according to the defects generated in the graphene film is shown in FIG. Referring to FIG. 11, it can be seen that the water droplets formed on the upper surface of the graphene film are larger in diameter compared to the graphene film without defects, and are opposite to the change tendency of the contact angle.
  • the reference diameter for the diameter may be set to 4.6 to 4.8 mm. Therefore, when the diameter of the water droplets formed on the upper surface of the graphene film is larger than 4.6 ⁇ 4.8mm it can be determined that a defect is generated in the graphene film.
  • the diameter of the water droplets may vary slightly depending on the amount of water to be sprayed, it is necessary to determine a reference value according to the amount of water.
  • the diameter of the water droplets is relatively small, such as 4.47 mm, and the height is 1.55 mm, but the diameter is larger and the height is lower toward the type 2, type 4, and type 6. You can see it losing.
  • the liquid spraying step (S20) is a step of forming water droplets by spraying water on the upper surface of the graphene film grown on the upper surface of the metal substrate.
  • a predetermined amount of water is sprayed onto the upper surface of the graphene film through the spraying nozzle 111 of the spraying nozzle unit 110 so that one droplet is formed.
  • the liquid spray step (S20) is to spray a liquid of 0.01 ⁇ 200 ⁇ l at a time so that one liquid droplet is formed. Therefore, in the liquid spraying step (S20), when a plurality of droplets are formed on the upper surface of the graphene film, the plurality of liquids are sprayed.
  • the liquid spraying step (S20) may be performed to simultaneously spray water at a position spaced apart from the upper surface of the graphene film in the width direction so that a plurality of water droplets are formed along the width direction of the graphene film.
  • the droplet may be formed in at least one along the width direction of the graphene film, a plurality of graphene film may be formed in accordance with the width.
  • the image information generating step (S30) is a step of generating image information on the shape of the water droplets formed on the upper surface of the graphene film. That is, the image information generating step S30 is a step of generating first image information on the plane of the droplet and second image information on the front image (rear or side image). In the image information generating step S30, the first photographing unit 121 generates first image information and the second photographing unit 125 generates second image information. The image information generating step S30 may be performed to selectively generate only one of the first image information and the second image information, and may be performed to generate both the first image information and the second image information.
  • the image information generating step (S30) is the first image information and / or the second image information is taken after the liquid droplet (c) is formed on the graphene film (b) and the shooting time interval of 3 to 30 seconds elapsed May be proceeded to.
  • the photographing time interval is set in consideration of the time required for the liquid droplet (c) to maintain a stable shape in the graphene film (b) and the transfer speed of the graphene film (b). If the shooting time interval is too short, the image may be taken before the liquid drop (c) is stabilized. In addition, if the shooting time interval is too long, the size of the liquid drop (c) may be reduced by evaporation of the liquid, depending on the type of liquid.
  • the shooting time interval may be longer than 30 seconds.
  • the image information generating step (S30) is to measure the diameter, height and contact angle of the liquid droplet (c) after measuring two or more times at intervals of shooting time in order to more accurately see the characteristics of the graphene film (b). It may be. This is because the liquid droplet (c) takes several seconds to stabilize while reacting with the surface of the graphene film (b).
  • the first image information is image information photographed from the upper surface of the water droplets, which is image information on the plane of the water droplets, and allows the diameter of the water droplets to be measured.
  • the second image information is image information photographed from the front, rear, or side of the water droplets.
  • the second image information is image information on the vertical shape of the water droplets, and the contact angle and height of the water droplets can be measured.
  • the image analysis step (S40) is a step of determining whether a defect is generated in the graphene film by calculating at least one of diameter, height, or contact angle with the graphene film from the image information on the droplet.
  • the image analyzing step S40 may use any one or both of the first image information and the second image information.
  • the image analyzing step (S40) is performed by extracting the shape of the droplet based on the brightness or the color of the droplet from the first image information or the second image information, and extracting the shape of the droplet from the extracted shape. At least one of the contact angles with the graphene film is calculated.
  • the image processing may be performed to more accurately display the outline with respect to the image information.
  • the image analyzing step (S40) is performed when the diameter of the droplet is larger than the reference diameter using at least one of the reference diameter, the reference height, and the reference contact angle for the preset droplet, the height of the droplet is lower than the reference height or It is determined that a defect is generated in the graphene film when the contact angle of is smaller than the reference contact angle.
  • the image analysis step (S40) may generate alarm information when at least one of the calculated diameter, height, or contact angle with the graphene film is out of the reference value.
  • the alarm signal generating step (S50) is a step of generating an alarm signal when any one value of the calculated diameter, height or contact angle with the graphene film is out of the reference value.
  • the image analyzer 130 generates alarm information and transmits the alarm information to the alarm unit 150 when any one of the calculated diameter, height, or contact angle with the graphene film is out of the reference value, and the alarm unit 150.
  • the alarm signal generating step S50 may generate an alarm signal when any one of the calculated diameter, height, or contact angle with the graphene film is out of the reference value, and at least two values are out of the reference value. In this case, an alarm signal can be generated.
  • the alarm signal generating step S50 does not proceed when the calculated diameter, height, or contact angle with the graphene film do not deviate from the reference value.
  • the drop removing step (S60) is a step of removing the water droplets sprayed on the upper surface of the graphene film.
  • the drop removing unit 160 is sprayed on the graphene upper surface when the region of the graphene film where the water droplets are finished, the image information generation is approaching close to the top surface of the graphene film by supplying wind, hot air or heat or irradiating light Remove the formed water droplets. Therefore, if it is determined that no defects are formed on the upper surface of the graphene film, the graphene film may be used as a normally produced product, and no loss occurs due to property inspection.
  • the graphene inspection device and method according to the present invention can be inspected in real time without transferring the graphene film with respect to the characteristics including whether a defect is present in the graphene film grown on the metal substrate.
  • the graphene inspection apparatus and method according to the present invention excludes defects that may occur in the process of transferring the graphene from the metal substrate and examines only the defects generated in the growth process, the roll-to-roll method by the chemical vapor deposition method It is possible to accurately identify and replace in real time whether or not a problem occurs in a large-scale graphene growth process that is grown with.
  • the graphene inspection apparatus and method according to the present invention can reduce the analysis time and lower the analysis cost compared to the existing method without using expensive equipment (Raman spectroscopy or transmission electron microscope, etc.).

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Abstract

La présente invention concerne un dispositif d'inspection de graphène et un procédé d'inspection de graphène utilisant celui-ci, le dispositif étant pour inspecter les propriétés d'un film de graphène comprenant la présence d'un défaut dans le film de graphène, et comprenant : une unité de buse de pulvérisation pour pulvériser un liquide sur la surface supérieure du film de graphène de manière à former une gouttelette de liquide ; une unité de génération d'informations d'image pour générer des informations d'image pour la forme de la gouttelette de liquide formée sur la surface supérieure du film de graphène ; et une unité d'analyse d'image pour calculer, à partir des informations d'image, au moins une valeur parmi le diamètre, la hauteur et l'angle de contact avec le film de graphène de liquide de manière à déterminer si un défaut est généré sur le film de graphène.
PCT/KR2017/000095 2016-01-05 2017-01-04 Dispositif et procédé d'inspection de graphène WO2017119715A1 (fr)

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CN110496304A (zh) * 2018-05-16 2019-11-26 富士胶片株式会社 微针阵列的制造方法
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CN109490567A (zh) * 2018-10-17 2019-03-19 重庆天泽新材料有限公司 玻璃纤维纱浸透速度检测方法
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CN110044279A (zh) * 2019-04-15 2019-07-23 华中科技大学 一种密封圈厚度测量装置及方法
CN110044279B (zh) * 2019-04-15 2020-05-19 华中科技大学 一种密封圈厚度测量装置及方法
CN110487679A (zh) * 2019-07-30 2019-11-22 武汉大学 一种测量液滴在固体表面摩擦力的装置
CN110487679B (zh) * 2019-07-30 2021-07-20 武汉大学 一种测量液滴在固体表面摩擦力的装置
CN110629191A (zh) * 2019-11-01 2019-12-31 北京大学 一种石墨烯薄膜卷对卷生产装置及方法

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