Measurement System

The measurement system addresses the challenge of real-time monitoring of conductivity, thickness, and topography during electrochemical coating by using probes, a computer, and imaging, enabling efficient optimization of the coating process.

JP7772770B2Active Publication Date: 2025-11-18トゥサシュテュルクハヴァジュルクヴェウザイサナイーアノニムシルケティ
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Patent Information

Application Number
JP2023501866
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2020-07-13
Filing Date
2021-04-14
Publication Date
2025-11-18
Estimated Expiration
2041-04-14

AI Technical Summary

Technical Problem

Existing technologies lack the ability to measure the change in electrical conductivity, thickness, and topographic profile of a substrate surface during the electrochemical coating process, making it difficult to optimize process parameters in real-time.

Method used

A measurement system comprising probes, a computer, and a movable arm to monitor conductivity and thickness of the coating in real-time, using current and voltage measurements, along with light reflection and imaging to assess surface topography, allowing for in-situ optimization of the coating process.

Benefits of technology

Enables real-time monitoring and optimization of the coating process by measuring conductivity, thickness, and topography, ensuring efficient and accurate application of process parameters without waiting for completion.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to an electrolytic vessel (2), at least one mandrel (3) contained in the vessel (2) and on which a coating (K) is formed by surface metallization, a liquid (S) contained in the vessel (2) and containing a solution capable of increasing the electrical conductivity of the mandrel (3), a plurality of probes (4) on the mandrel (3) capable of measuring the electrical conductivity of the mandrel (3), at least one first set of probes (4a) capable of transmitting an electrical current on the mandrel (3) and measuring the current flowing on the mandrel (3) by means of an ammeter (A) arranged thereon, and at least one second set of probes (4b) capable of measuring a voltage difference by means of a voltmeter (V).
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Description

[Technical Field]

[0001] The present invention relates to a measurement device used in a surface metallization process. [Background technology]

[0002] Electrochemical coatings can be applied in the form of electroplating or electroless plating. Electroless plating is formed by obtaining atoms through autocatalytic chemical reduction without the use of electric current, while electroplating is formed by electrolysis. Electrolysis is a process in which chemical compounds dissolved in a liquid are dissociated using an electric current. Electrolysis takes place in a vessel called an electrolytic vessel or cell. Two electrodes, not in contact with each other, are immersed in the vessel containing the dissolved compounds (electrolyte), causing them to dissociate into positively and negatively charged ions. When the electrodes are connected to a current source, a potential difference (electric field) is created, causing the ions to migrate toward the oppositely charged electrode (pole). Positively charged ions migrate to the cathode (negative electrode), while negatively charged ions flow toward the anode (positive electrode). Atoms oxidized at the anode surface travel in an ionized state in solution and are reduced at the cathode surface. This results in a surface metallization (or electrolytic coating) process. Electrolytic coating has advantages such as improving the surface's wear resistance, corrosion resistance, and electrical conductivity, and is therefore widely used.

[0003] The process of imparting electrical conductivity is carried out in various chemical solutions on substrates that are non-conductive and / or have a conductivity below the desired value. The thickness of the coating formed by the atoms attached to the surface varies depending on the coating parameters (temperature, time, current density, current source, pH, mixture, etc.), bath chemistry, and composition. Therefore, being able to measure the change in electrical conductivity of the substrate surface during the coating process is important for better interpreting the mechanism of the study and for measuring the conductivity obtained at each step. Furthermore, measuring the thickness and topographic profile of the coating formed by the atoms attached to the surface at different temperatures during each stage of the process plays an important role in determining the parameters to be applied in the different steps.

[0004] U.S. Patent No. 7,078,919 (US7,078,919B2), a U.S. patent document included in the prior art, discloses a method for determining the resistance profile of a PN structure or a silicon surface layer on an SOI. The method involves passing an anodic current through a test site to oxidize the isolated layer and measuring the resistance of the isolated layer by a four-point probe or Van der Pauw method. The sheet resistance of the test area is measured in situ.

[0005] German patent application DE 2902150 A1, which is included in the prior art, discloses an apparatus for measuring the surface conductivity of a conductive sheet on an insulating material. The apparatus has two measuring wheels that apply pressure to the sheet and are connected to opposite poles of a measuring current source. The wheels are mounted so that they rotate about an axis perpendicular to the axis of the sheet. Summary of the Invention

[0006] The measurement system developed by this invention allows for coating property measurements at each step of the surface metallization process carried out in solution. During coating, it is possible to measure the change in electrical conductivity of the substrate surface, determine the surface thickness profile, and monitor the topographic profile formed on the surface by atoms deposited on the substrate at each step of the coating process. This allows for observation of the coating efficiency and the accuracy of the process parameters. Therefore, the coating process can be optimized by changing the process parameters in situ, without waiting for the process to finish.

[0007] The object of the present invention is achieved by a measurement system, as defined in claim 1 and the claims dependent thereon, comprising an electrolytic vessel, at least one mandrel contained in the electrolytic vessel and coated with a surface metallization, a liquid contained in the electrolytic vessel and containing a solution capable of increasing the electrical conductivity (conductivity) of the mandrel, a plurality of probes on the mandrel allowing measurement of the electrical conductivity of the mandrel, at least one first probe set capable of transmitting an electrical current on the mandrel, the current flowing on the mandrel being measured by an ammeter provided on the first probe set, and at least one second probe set allowing measurement of a voltage difference by a voltmeter.

[0008] The measurement system of the present invention comprises a computer that allows for the calculation of a coating conductivity value in real time using measurements of current and voltage that change during the surface metallization process, and at least one arm that allows the probe to move closer to or farther from the mandrel by approximately the same amount as the thickness of the coating increases or decreases on the mandrel.

[0009] In one embodiment of the present invention, the measurement system comprises a probe that is substantially completely covered with an insulating material that prevents contact with the liquid.

[0010] In one embodiment of the present invention, the measurement system includes at least one chamber connected to a power source, an arm connected to the chamber that can be automatically moved toward or away from the mandrel by a computer, and a voltmeter located within the chamber.

[0011] In one embodiment of the present invention, the measurement system includes a computer that issues a warning message that the surface metallization process should be stopped when the mandrel reaches a user-defined conductivity.

[0012] In one embodiment of the present invention, the measurement system includes a mandrel that is non-conductive or has a conductivity (conductivity) below a user-desired value prior to the surface metallization process.

[0013] In one embodiment of the present invention, the measurement system comprises at least one light source capable of transmitting long wavelength light onto the coating during surface metallization, at least one detector that captures reflected light from the coating, and a computer that enables thickness determination to be made using data received from the detector.

[0014] In one embodiment of the present invention, the measurement system comprises a detector, the curved structure of which allows all the light rays reflected from the coating to be collected on the detector itself.

[0015] One embodiment of the present invention includes at least one camera that captures and scans light reflected from the coating, and a computer that enables the surface topography of the coating to be measured using data received from the camera.

[0016] In one embodiment of the present invention, the measurement system includes a computer that simultaneously analyzes the conductivity measurement using the measurement data received from the probe and the thickness measurement using the measurement data received from the detector, thereby also determining a thickness value when a user-determined conductivity value is reached.

[0017] In one embodiment of the present invention, the measurement system comprises a computer that allows to perform Van der Pauw and / or four-point measurements in liquids containing different ions and at temperatures different from room temperature.

[0018] A measurement system realised to achieve the objects of the invention is shown in the accompanying figures, of which reference will now be made. [Brief explanation of the drawings]

[0019] [Figure 1] FIG. 1 is a schematic diagram of a measurement system for conducting conductivity measurements. [Figure 2] FIG. 2 is a schematic diagram of a measurement system for conducting conductivity measurements. [Figure 3] FIG. 3 is a schematic diagram of a measurement system for measuring the thickness of a coating. [Figure 4] FIG. 4 is a schematic diagram of a measurement system for measuring the topography of a coating. DETAILED DESCRIPTION OF THE INVENTION

[0020] The measurement system (1) comprises an electrolytic vessel (2), at least one mandrel (3) housed in the electrolytic vessel (2) and on which a coating (K) is formed by surface metallization, a liquid (S) housed in the electrolytic vessel and containing a solution capable of increasing the electrical conductivity of the mandrel (3), and a plurality of probes (4) on the mandrel (3) that enable measurement of the electrical conductivity of the mandrel (3), including at least one first probe set (4a) and at least one second probe set (4b) that enable measurement of a voltage difference by a voltmeter (V) (FIG. 1). The at least one first probe set (4a) enables transmission of a current onto the mandrel (3), and the current flowing through the mandrel (3) can be measured by an ammeter (A) disposed on the first probe set (4a).

[0021] The measurement system (1) of the present invention comprises a computer (5) that allows the electrical conductivity value of the coating (K) to be calculated in real time using measurements of the current and voltage that change during the surface metallization process (FIG. 2), and at least one arm (6) that allows the probe (4) to be moved closer to or farther away from the mandrel (3) by approximately the same amount as the thickness of the coating (K) increases or decreases on the mandrel (3).

[0022] The process of imparting electrical conductivity is carried out by applying a surface metallization to an insulating and / or poorly conductive mandrel (3). The conductivity of the mandrel (3) is measured using four probes (4). The first set of probes (4a) allows a current to flow through the mandrel. The current is measured by an ammeter (A). The second set of probes (4b) is used to measure the voltage. The voltage difference generated between the second set of probes (4b) is measured by a voltmeter (V).

[0023] To measure the conductivity gained at each step of the surface metallization, a probe (4) positioned on a mandrel (3) must be moved as the coating thickness increases. A single arm (6) allows the probe (4) to move closer to or further away from the mandrel (3) by an amount roughly equal to the increase or decrease in the coating (K) thickness on the mandrel (3). The current and voltage values ​​that change during coating are calculated in real time by a computer (5) using the formula ρ = V × A / (I × d) for resistance and σ = 1 / ρ for conductivity. In this formula, ρ (rho) represents resistivity, A represents the surface area of ​​the sample, I represents current, d represents the distance between the probes, and σ (sigma) represents conductivity. The measured data for the coating (K) can be recorded in the computer and compared with previous applications. The recorded values ​​of the coating (K) conductivity and / or thickness allow monitoring the performance and quality of the measurement system (1) operation.

[0024] In one embodiment of the present invention, the measurement system 1 includes a probe 4 that is almost completely coated with an insulating material to prevent contact with the liquid S. The outer layer of the probe 4 is coated with the insulating material to prevent measurement of the conductivity of the liquid S. The portion of the probe 4 that contacts the mandrel 3 is free of the insulating material, allowing measurement of only the coating characteristics of the mandrel 3.

[0025] In one embodiment of the present invention, the measurement system (1) comprises at least one chamber (7). The chamber (7) is connected to a power supply (E), and an arm (6) is connected to the chamber (7), with a voltmeter (V) located within the chamber (7). The arm (6) can be automatically moved toward or away from the mandrel (3) by a computer (5). The arm (6), which moves according to an algorithm in the computer (5), is connected to the chamber (7), ensuring that the probe (4) moves as the thickness of the coating (K) on the mandrel (3) increases.

[0026] In one embodiment of the present invention, in the measurement system (1), the computer (5) issues a warning message that the surface metallization process must be stopped when a conductivity of the mandrel determined by the user prior to the electrolysis process is reached.

[0027] In one embodiment of the present invention, the measurement system (1) includes a mandrel (3) that is non-conductive or has a conductivity below a user-desired value prior to a surface metallization process, whereby electrical conductivity is imparted to the insulating and / or poorly conductive mandrel (3) by allowing different atoms to be deposited on the surface in multiple steps.

[0028] In one embodiment of the present invention, the measurement system (1) comprises at least one light source (8) that transmits long-wavelength light onto the coating (K) during surface metallization, at least one detector (9) that captures reflected light from the coating (K), and a computer (5) that can determine thickness using data received from the detector (9). During the surface metallization process, the thickness of the coating (K) is measured in situ at different temperatures while the mandrel (3) is immersed in the liquid (S). After the initial thickness of the mandrel (3) is calibrated, long-wavelength light is transmitted and a detector (9) that can capture all reflected light from the mandrel (3) is used. Using the data obtained from the detector (9), the thickness increase can be monitored by an algorithm in the computer (5). In this way, the thickness of the coating (K) can be monitored as it changes during the surface metallization process, allowing the coating efficiency and the accuracy of the process parameters to be monitored and optimized without waiting for the process to be completed (FIG. 3).

[0029] In one embodiment of the present invention, the measurement system 1 includes a detector 9 having a curved structure, which increases the surface area of ​​the detector 9, which captures light of long wavelengths, and improves measurement accuracy.

[0030] In one embodiment of the present invention, the measurement system (1) comprises at least one camera (10) for capturing and scanning the reflected light from the coating (K) and a computer (5) for measuring the surface topography of the coating (K) using the data received from the camera (10). Checking the roughness of the coating (K) and obtaining a surface map allows checking the desired roughness values ​​at different temperatures during the surface metallization process. Furthermore, this measurement is performed by contactless scanning of the mandrel (3) surface in a liquid medium during the coating process, allowing for efficient monitoring of coating efficiency and process parameters (Figure 4).

[0031] In one embodiment of the present invention, the measurement system (1) includes a computer (5) that simultaneously analyzes conductivity measurements using data received from the probe (4) and thickness measurements using data received from the detector (9). This allows a thickness value to be determined when a user-defined conductivity value is reached. Once the desired conductivity value is reached, the thickness measurement is stopped and the current thickness value is used as the coating thickness.

[0032] In one embodiment of the present invention, the measurement system (1) is equipped with a computer (5) that enables Van der Pauw and / or four-point measurements to be performed in a liquid (S) containing different ions and at temperatures different from room temperature. Surface metallization includes alkaline cleaning, acid etching, sensitization, and activation processes. During these operations, the composition and temperature of the bathroom change. During the surface metallization process, the temperature of the solution can be adjusted using a hot plate equipped with a magnetic stirrer. Temperature can be controlled and maintained constant using a thermometer or thermocouple. In the measurement system (1) where these processes are performed, the computer (5) measures the resistance of the mandrel (3) in solutions containing multiple liquids (S) at different temperatures, providing the measurement system (1) with flexible operating conditions. This allows for real-time observation of coating properties during the process.

[0033] All parts in the figures are individually referenced by numerals, and the corresponding terms for these numerals are given below. [Explanation of symbols]

[0034] 1. Measurement System 2 Electrolytic vessel 3 mandrels 4 Probes 4a First probe set 4b Second probe set 5. Computer 6 Arm 7 Chamber 8 light source 9 Detector 10 Camera (S) Liquid (A) Ammeter (V) Voltmeter (K) Coating (E) Power supply

Claims

1. an electrolytic vessel (2); at least one mandrel (3) accommodated in the electrolytic vessel (2) and on which a coating (K) is formed by surface metallization; a liquid (S) contained in the electrolytic vessel and containing a solution capable of increasing the conductivity of the mandrel (3); a plurality of probes (4) on the mandrel (3) that allow measurement of the conductivity of the mandrel (3); At least one chamber (7) in which a voltmeter (V) and an ammeter (A) are arranged; at least one arm (6) connected to said at least one chamber (7); at least one light source (8) capable of transmitting long wavelength light onto said coating (K) during said surface metallization; At least one detector (9) for capturing reflected light from said coating (K); a computer (5); Equipped with The plurality of probes (4) at least one first set of probes (4a) making it possible to transmit an electric current on the mandrel (3), the electric current flowing on the mandrel (3) being measurable by the ammeter (A) connected to said first set of probes (4a); at least one second set of probes (4b) that allows measurement of a voltage difference on the mandrel (3), the voltage difference on the mandrel (3) being measurable by the voltmeter (V) connected to the second set of probes (4b); The computer (5) receiving and recording measurements of the current and voltage of the coating (K) that change during the surface metallization process, as measured by the ammeter (A) and the voltmeter (V); It is configured to calculate the value of the conductivity of the coating (K) in real time by comparing the measured value with a previous application, the computer (5) is configured to receive data of the reflected light detected by the detector (9) and use the data to detect in real time the thickness of the coating (K) increasing or decreasing on the mandrel (3); The computer (5) moves the chamber connected to the at least one arm (6) by automatically moving the at least one arm (6) closer to or away from the mandrel (3) based on the thickness of the coating (K) detected in real time, thereby moving the multiple probes (4) connected to the ammeter (A) and the voltmeter (V) in the chamber away from the mandrel (3) by an amount equal to the increase in the thickness of the coating (K) detected in real time, or closer to the mandrel (3) by an amount equal to the decrease in the thickness of the coating (K) detected in real time. This measurement system (1)

2. 2. The measuring system (1) according to claim 1, wherein the probe (4) is covered with an insulating material that prevents contact with the liquid (S) except for the part configured to be in contact with the mandrel (3).

3. 3. The measuring system (1) according to claim 1 or 2, wherein the at least one chamber (7) is connected to a power source (E).

4. 4. The measuring system (1) according to claim 1, wherein the computer (5) issues a warning message that the surface metallization process must be stopped when the conductivity of the mandrel (3) reaches a user-defined conductivity.

5. 5. The measuring system (1) according to any one of claims 1 to 4, wherein the mandrel (3) is non-conductive or has a conductivity below a user-desired value prior to the surface metallization process.

6. 2. The measuring system (1) according to claim 1, wherein the detector (9) has a curved structure, which allows all reflected light from the coating (K) to be collected on the detector itself.

7. at least one camera (10) for scanning light reflected from said coating (K); 7. The measuring system (1) according to any one of claims 1 to 6, wherein the computer (5) makes it possible to measure the surface topography of the coating using data received from the camera (10).

8. 8. The measuring system (1) according to any one of claims 5 to 7, wherein the computer (5) simultaneously analyzes the conductivity measurement of the coating (K) using the data received from the probe (4) and the thickness measurement of the coating (K) using the data received from the detector (9), thereby being able to determine a thickness value when a user-defined conductivity value is reached.

9. 9. The measuring system (1) according to claim 1, wherein the computer (5) is capable of carrying out Van der Pauw and / or four-point measurements in the liquid (S) containing different ions at temperatures different from room temperature.

Citation Information

Patent Citations

  • Iron oxide layer inspecting apparatus and method

    JP2003194780A

  • In-situ profile measurement in electroplating process

    JP2006328537A

  • In situ determination of resistivity, mobility and dopant concentration profiles

    US20050052191A1

  • Deposition of thin electroconductive polymer film of desired resistance for gas sensing applications

    WO1998011279A1