CN112857624B - Measuring device for stress in coating and operation method - Google Patents

Measuring device for stress in coating and operation method Download PDF

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CN112857624B
CN112857624B CN202110004916.4A CN202110004916A CN112857624B CN 112857624 B CN112857624 B CN 112857624B CN 202110004916 A CN202110004916 A CN 202110004916A CN 112857624 B CN112857624 B CN 112857624B
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cathode
internal stress
liquid level
computer
coating
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CN112857624A (en
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张津
杨竞涵
焦进超
徐伟生
丁啸云
连勇
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University of Science and Technology Beijing USTB
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00Measuring force or stress, in general
    • G01L1/02Measuring force or stress, in general by hydraulic or pneumatic means
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00Processes for servicing or operating cells for electrolytic coating
    • C25D21/12Process control or regulation

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  • Chemical & Material Sciences (AREA)
  • Automation & Control Theory (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Electroplating Methods And Accessories (AREA)

Abstract

The invention provides a device for measuring the internal stress of a coating and an operation method, belonging to the technical field of internal stress detection. The device includes: the power supply device is used for providing voltage for electroplating; the electroplating device comprises a plating bath, an anode plate, a cathode and the like; the automatic temperature control device comprises a temperature control box, a heating pipe, a thermocouple and the like, and provides a constant temperature environment for the plating solution and the working solution; the stress measuring device comprises a working cavity, a capillary tube and the like; a support; the camera monitors the liquid level scale of the capillary; and the computer automatically reads the scale change value of the liquid level of the capillary in the picture provided by the camera, converts the electric signal into an internal stress value through software processing, and finally displays the internal stress value as a curve of the plating layer internal stress changing along with time. The invention has simple structure, convenient carrying, simple and convenient operation, accurate detection result and no damage to the plating layer.

Description

Measuring device for stress in coating and operation method
Technical Field
The invention relates to the field of internal stress detection, in particular to a measuring device and an operating method for the internal stress of a coating.
Background
The metal member is applied to the industries of precision instruments, chemical engineering, transportation, weapons, aerospace, atomic energy and the like, can be corroded by corrosive media in certain environments, and people can carry out electroplating or chemical plating treatment on the surface of the material, so that the treated material has wider application. Along with the expansion of the application range of electroplating in various fields of national economy, higher and higher requirements are put forward on the performance of electroplated layers. The coating may crack, bubble or peel, or even deform due to the presence of internal stresses in the coating, which may also reduce the fatigue strength of the substrate, causing stress corrosion of the coating, which all adversely affect the properties of the coating. Where mechanical properties are often particularly desired, the internal stresses in the coating are as low as possible. Therefore, it is very necessary to accurately measure the internal stress of the plating layer in the field of electroplating.
The conventional methods for measuring the internal stress of the coating mainly comprise a cathode test piece bending deformation method, a cathode test piece length deformation method, a spiral tube cathode deformation method, a resistance strain method and the like.
The cathode test piece bending deformation method is realized by bending a cathode thin sheet towards an anode or a back anode by means of internal stress and measuring the displacement of a free end, but each thin sheet sample can only obtain one stress data, so that the research on the relation between the stress and the thickness of a coating is inconvenient; the principle of the cathode test piece length deformation method is that the length of a thin cathode is changed by internal stress, the internal stress of a coating is obtained by measuring the length variation of a free end, although the length variation is easy to measure, the internal stress is loosened by the change of the length, and the experimental result is influenced.
The principle of the spiral tube cathode deformation method is based on the change of curvature radius when a spiral sample is electroplated, although continuous reading can be carried out, the internal stress of a thin plating layer cannot be measured; the resistance strain method is to measure the internal stress of a plating layer by utilizing the principle that the resistance wire changes in resistance value due to expansion and contraction, although the stress change condition in the electroplating process can be continuously reflected, the surface of a sample to which a strain gauge is attached is coated with insulating paint and naturally dried, so that the experiment can be started, and the early preparation time is long.
Disclosure of Invention
The invention provides a measuring device for the internal stress of a coating and an operation method thereof, aiming at the defects of the existing method for measuring the internal stress of the coating. The invention utilizes metal to plate on the negative pole, the internal stress is produced in the plating layer when plating, based on the principle that the negative pole forms symmetrical deflection around the vertical axis, the volume change in the working cavity is caused, and then the change of the liquid level scale of the capillary tube is caused, the camera monitors the liquid level of the capillary tube in real time, and the internal stress of the plating layer is calculated by a Stoney formula, and the internal stress of the plating layer is converted into a change curve of the internal stress of the plating layer through software processing.
A measuring device of the internal stress of a coating is characterized in that: the device comprises a power supply device, an electroplating device, an automatic temperature control device, a stress measuring device, a camera, a bracket and a computer;
the electroplating device comprises a plating tank, a cathode, an anode plate, an electrode plate and a slide rail; the anode plate is fixed through the electrode plate, the lower end of the anode plate is arranged in the plating solution, the electrode plate is arranged on the slide rails on the two sides of the plating tank, and the distance between the anode plate and the cathode is adjusted through sliding the electrode plate to achieve the best electroplating effect;
the automatic temperature control device comprises a temperature control box, a heating pipe and a thermocouple;
the stress measuring device comprises a working cavity, a capillary tube, a cavity base, a clamping groove, a flashboard switch, a cover plate, a fluid infusion port, an elastic device, a contact point groove, a contact point, a spring groove, a thread, a baffle, a sliding block and an annular flat gasket; the cathode is pressed on one side of the working cavity through the cover plate and is connected with the power supply device, and the capillary tube is connected with the working cavity. The heating pipe and the thermocouple in the plating bath and the working cavity are connected with a temperature control box; can prevent the error of the plating stress caused by the temperature change at the two sides of the cathode. A clamping groove, a flashboard, an annular flat gasket and a springing device are arranged between the working cavity and the cover plate, one side of the flashboard is close to the working liquid, the clamping groove is used for placing a cathode, the springing device is fixed in the spring groove when in a compressed state, one end of the springing device is connected with the spring groove, and the other end of the springing device is embedded in the annular flat gasket; the spring groove, the flashboard and the working cavity are tightly connected in a mode of welding and bonding a cross-linking agent.
Further, the cavity base is connected with the working cavity in a mode including threaded connection. And the cavity base has specifications with different lengths, and can be correspondingly adjusted according to the depth of the plating solution.
Further, the measuring device can detect the thickness of the cathode in the range of 0.01-0.5mm and can detect the internal stress of the coating with the coating thickness of more than 1 μm.
Further, in order to improve the use efficiency of the measuring device, the cathode needs to be rapidly clamped; the method for rapidly clamping the cathode comprises the following steps:
(1) firstly, closing the flashboard through the flashboard switch to prevent working liquid from flowing out, and pulling the cover plate to enable the elastic device to be in a stretching state;
(2) the cathode is placed in the clamping groove, the cover plate is pressed back to enable the elastic device to be in a compressed state, and the contact point is tightly connected with the contact point groove through the magnetism of the contact point groove and the contact point;
(3) and opening the flashboard, enabling working solution to flow in and contact with the cathode, and completing the rapid clamping of the cathode.
An operating method for measuring the internal stress of a coating by using the device comprises the following steps: (1) setting the temperature of the plating solution and the working solution, starting a camera and a computer, adjusting the plate electrode to a proper distance, and setting the photographing time interval of the camera;
(2) preparing a cathode for pretreatment, quickly clamping, checking whether the working solution is full through a solution supplementing port, respectively connecting an anode plate and the cathode with the anode and the cathode of a power supply device, starting the power supply device, setting current parameters, and starting electroplating;
(3) when the side of the cathode, which is in contact with the plating solution, is plated, the cathode is bent by internal stress generated by the plating layer, so that the internal volume of the working cavity is changed, the liquid level in the capillary tube rises or falls, the camera takes pictures of the liquid level scale of the capillary tube and transmits the pictures to the computer, the computer reads and identifies the pictures, and the front and back readings of the liquid level of the capillary tube are obtained, so that the change of the liquid level of the capillary tube is monitored, and the change curve of the internal stress of the plating layer along with the time is displayed on the computer after the processing of a software system.
Further, the camera shoots the scales where the liquid level is located in the capillary, the shooting time difference can be correspondingly adjusted according to the electroplating speed, the picture is transmitted to the computer, the computer identifies the picture and reads the liquid level scales, and the liquid level variation is monitored through the capillary liquid level scales of adjacent pictures.
Further, the method for calculating the internal stress of the plating layer comprises the following steps: firstly, a computer identifies a picture transmitted by a camera to read the liquid level variation of the capillary tube, and the liquid level variation is based on a Stoney formula:
σ=EsT2/6Rt (1)
wherein σ is the internal stress of the plating layer, EsThe Young's modulus of the cathode, T the thickness of the cathode, T the thickness of the coating and R the radius of curvature of the cathode.
And (4) carrying out further derivation, and carrying out data processing and calculation through a software system of a computer, and finally solving the internal stress of the corresponding plating layer.
Furthermore, the computer is used for controlling starting, the sliding distance of the electrode plate, photo transmission and recognition and signal acquisition, and carrying out data conversion and processing on the electric signals to finally convert the electric signals into stress change curves.
Preferably, the device comprises a software system including signal acquisition control, data storage, processing and analysis, electrode plate displacement control, analysis result output and the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention has simple structure, convenient carrying and simple and convenient operation, and does not damage and destroy the plating layer; meanwhile, the stress measuring device is suitable for cathodes in various shapes and different plating species such as electroplating, chemical plating and the like;
(2) according to the invention, after the cathode pretreatment is finished, the exposure time of the cathode in the air is shortened, the electroplating performance is improved, and the accuracy of measuring the internal stress of the coating is improved through the rapid clamping of the cathode;
(3) in the invention, one side of the cathode is contacted with the working solution, so that insulating paint does not need to be coated on the back surface of the cathode, and a great deal of time is saved for preparation work before plating;
(4) the invention can measure the internal stress of the thinner plating layer, can obtain the continuous change curve of the internal stress instead of a single stress value while ensuring higher measurement precision, and is convenient for researching the change of the internal stress of the plating layer along with time.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention, illustrate embodiments of the invention and together with the description serve to explain the invention and are not to limit the invention.
FIG. 1 is a schematic diagram of the overall structure of the device for measuring the internal stress of the coating.
Fig. 2 is a schematic structural diagram of a stress measuring device.
Fig. 3 is a schematic cross-sectional view of a stress measuring device (with the springing device in tension).
Fig. 4 is a schematic drawing of the shutter in plan and partially in section.
The labels in the figure are respectively: 1-power supply device, 2-computer, 3-coating bath, 4-cathode, 5-anode plate, 6-temperature control box, 7-1-heating tube a, 7-2-heating tube b, 8-1-thermocouple a, 8-2-thermocouple b, 9-working cavity, 10-capillary tube, 11-cavity base, 12-camera, 13-support, 14-electrode plate, 15-slide rail, 16-clamping groove, 17-flashboard, 18-flashboard switch, 19-cover plate, 20-liquid supplementing port, 21-elastic device, 22-contact point groove, 23-contact point, 24-spring groove, 25-thread, 26-baffle plate, 27-slide block and 28-annular flat pad.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
The invention provides a device and a method for measuring the stress in a coating.
As shown in fig. 1 and fig. 2, the device for measuring the internal stress of the coating comprises a power supply device 1, an electroplating device, an automatic temperature control device, a stress measuring device, a camera 12, a bracket 13 and a computer 2; the electroplating device comprises a plating bath 3, a cathode 4, an anode plate 5, an electrode plate 14 and a slide rail 15, the automatic temperature control device comprises a temperature control box 6, a heating pipe a7-1, a heating pipe b7-2, a thermocouple a8-1 and a thermocouple b8-2, the stress detection device comprises a working cavity 9, a capillary tube 10, a cavity base 11, a clamping groove 16, a flashboard 17, a flashboard switch 18, a cover plate 19, a liquid supplementing port 20, an elastic device 21, a contact point groove 22, a contact point 23, a spring groove 24, a thread 25, a baffle 26, a slide block 27 and an annular flat pad 28; the anode plate 5 is fixed by an electrode plate 14, the lower end of the anode plate is arranged in the plating solution, and the electrode plate 14 is arranged on slide rails 15 at two sides of the plating tank 3, so that the distance between the anode plate 5 and the cathode 4 can be conveniently adjusted; the cathode 4 is pressed on one side of the working cavity 9 through the cover plate 19 and is connected with the power supply device 1, the capillary tube 10 is connected with the working cavity 9, the coating bath 3, the heating pipe a7-1 and the heating pipe b7-2 in the working cavity 9, the thermocouple a8-1 and the thermocouple b8-2 are connected with the temperature control box 6.
As shown in fig. 3, a clamping groove 16, a gate plate 17, an annular flat pad 28 and an elastic device 21 are arranged between the working cavity 9 and the cover plate 19, one side of the gate plate 17 is close to the working fluid, the clamping groove 16 is used for placing the cathode 4, the elastic device 21 is fixed in the spring groove 24 when in a compressed state, one end of the elastic device 21 is connected with the spring groove 24, the other end of the elastic device is embedded in the annular flat pad 28, and the spring groove 24, the gate plate 17 and the working cavity 9 are tightly connected in a manner of containing welding and bonding a cross-linking agent.
As shown in fig. 4, which is a schematic plan view and a partial sectional view of the shutter 17, the shutter 17 includes a plurality of shutters 26 inside, a slider 27 at a top end of each shutter 26 is connected to the shutter switch 18 through a spring, and the shutter switch 18 is slid to move the shutters 26 forward and backward by the spring, so as to close and open the shutter 17.
The following description is given with reference to specific examples.
Example 1
A round sample made of red copper material and having a thickness of 0.5mm and a diameter of 30mm is used as a cathode 4, the Watt nickel is electroplated, and a change curve of the internal stress of a plating layer in the process of electroplating the Watt nickel is measured.
(1) Setting the temperature of the plating solution and the working solution at 55 ℃, starting the camera 12 and the computer 2, adjusting the electrode plate 14 to enable the distance between the anode plate 5 and the cathode 4 to be 5cm, setting the photographing time interval of the camera 12 to be 0.5s, and preparing the red copper sample for pretreatment;
(2) rapidly clamping the sample, checking whether the working solution is full from the solution supplementing port 20, respectively connecting the anode plate 5 and the cathode 4 with the anode and the cathode of the power supply device 1, starting the power supply device 1, setting the current to be 0.2A, and setting the electroplating time to be 20 min;
(3) the matrix is deformed by the internal stress generated by electroplating, the liquid level of the capillary 10 is monitored by the camera 12, and the change curve of the internal stress of the nickel-plated layer along with the electroplating time is displayed on the computer 2 after the processing of a software system. Compared with the experimental result obtained by a resistance strain method, the error range is within 0.5 percent, so that the method has higher accuracy in measuring the internal stress of the plating layer.
Example 2
A square sample with the thickness of 0.1mm and the side length of 40mm, which is made of a steel material, is used as a cathode 4, hexavalent chromium is electroplated, and a change curve of the internal stress of a plating layer in the process of electroplating chromium is measured.
(1) Setting the temperature of the plating solution and the working solution at 50 ℃, starting the camera 12 and the computer 2, adjusting the electrode plate 14 to enable the distance between the anode plate 5 and the cathode 4 to be 4.5cm, setting the photographing time interval of the camera 12 to be 0.5s, and preparing a steel sample for pretreatment;
(2) rapidly clamping the sample, checking whether the working solution is full from the solution supplementing port 20, respectively connecting the anode plate 5 and the cathode 4 with the anode and the cathode of the power supply device 1, starting the power supply device 1, setting the current to be 0.4A, and setting the electroplating time to be 40 min;
(3) the matrix is deformed by the internal stress generated by electroplating, the liquid level of the capillary 10 is monitored by the camera 12, and the change curve of the internal stress of the chromium coating along with the electroplating time is displayed on the computer 2 after the processing of a software system. Compared with the experimental result obtained by an X-ray diffraction method, the error range is within 1.0 percent, so that the method for measuring the internal stress of the coating has higher accuracy.
Example 3
A plastic round material sample with the thickness of 0.05mm and the diameter of 25mm is used for carrying out chemical copper plating, and the change curve of the internal stress of a plating layer in the chemical copper plating process is measured.
(1) Setting the temperature of the plating solution and the working solution to be 45 ℃, starting the camera 12 and the computer 2, setting the photographing time interval of the camera 12 to be 0.5s, and preparing the plastic sample for pretreatment;
(2) rapidly clamping the sample, checking whether the working solution is full from the solution supplementing opening 20 without starting the power supply device 1 or connecting the anode and the cathode of the power supply device 1, and electroplating for 50 min;
(3) the matrix is deformed by the internal stress generated by chemical plating, the liquid level of the capillary 10 is monitored by the camera 12, and the change curve of the internal stress of the copper plating layer along with the chemical plating time is displayed on the computer 2 after the processing of a software system. Compared with the experimental result obtained by an X-ray diffraction method, the error range is within 1.5 percent, so that the method for measuring the internal stress of the coating has higher accuracy.
Finally, it should be noted that: although the present invention has been described in detail in the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents may be made in the embodiments described above, or some features may be substituted for those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (8)

1. A measuring device of the internal stress of a coating is characterized in that: the device comprises a power supply device, an electroplating device, an automatic temperature control device, a stress measuring device, a camera, a bracket and a computer;
the electroplating device comprises a plating tank, a cathode, an anode plate, an electrode plate and a slide rail; the anode plate is fixed through a plate electrode, the lower end of the anode plate is arranged in the plating solution, and the plate electrode is arranged on slide rails on two sides of the plating tank, so that the distance between the anode plate and the cathode can be conveniently adjusted;
the automatic temperature control device comprises a temperature control box, a heating pipe and a thermocouple;
the stress measuring device comprises a working cavity, a capillary tube, a cavity base, a clamping groove, a flashboard switch, a cover plate, a fluid infusion port, an elastic device, a contact point groove, a contact point, a spring groove, a thread, a baffle, a sliding block and an annular flat gasket; the cathode is tightly pressed on one side of the working cavity through the cover plate and is connected with the power supply device, and the capillary tube is connected with the working cavity; the heating pipe and the thermocouple in the plating bath and the working cavity are connected with a temperature control box; a clamping groove, a flashboard, an annular flat gasket and a springing device are arranged between the working cavity and the cover plate, one side of the flashboard is close to the working liquid, the clamping groove is used for placing a cathode, the springing device is fixed in the spring groove when in a compressed state, one end of the springing device is connected with the spring groove, and the other end of the springing device is embedded in the annular flat gasket; the spring groove, the flashboard and the working cavity are tightly connected in a mode of welding and bonding a cross-linking agent;
the camera shoots the capillary liquid level scales before and after the change in real time and transmits the pictures to the computer, and the computer reads and identifies the pictures to obtain a change curve of the internal stress of the plating layer along with time.
2. The apparatus for measuring in-coating stress according to claim 1, wherein: the cavity base is connected with the working cavity in a mode including threaded connection, and the cavity base has specifications with different lengths and can be correspondingly adjusted according to the depth of the plating solution.
3. The apparatus for measuring in-coating stress according to claim 1, wherein: the measuring device is capable of detecting a thickness of the cathode in the range of 0.01-0.5 mm.
4. The apparatus for measuring in-coating stress according to claim 1, wherein: in order to improve the use efficiency of the measuring device, the cathode needs to be rapidly clamped; the method for rapidly clamping the cathode comprises the following steps:
(1) firstly, closing the flashboard through the flashboard switch to prevent working liquid from flowing out, and pulling the cover plate to enable the elastic device to be in a stretching state;
(2) the cathode is placed in the clamping groove, the cover plate is pressed back to enable the elastic device to be in a compressed state, and the contact point is tightly connected with the contact point groove through the magnetism of the contact point groove and the contact point;
(3) and opening the flashboard, enabling working solution to flow in and contact with the cathode, and completing the rapid clamping of the cathode.
5. A method of operating a device for measuring stresses in a coating as claimed in claim 1, characterized in that: comprises the following steps:
(1) setting the temperature of the plating solution and the working solution, starting a camera and a computer, adjusting the plate electrode to a proper distance, and setting the photographing time interval of the camera;
(2) preparing a cathode for pretreatment, quickly clamping, checking whether the working solution is full through a solution supplementing port, respectively connecting an anode plate and the cathode with the anode and the cathode of a power supply device, starting the power supply device, setting current parameters, and starting electroplating;
(3) when the side of the cathode, which is in contact with the plating solution, is plated, the cathode is bent by internal stress generated by the plating layer, so that the internal volume of the working cavity is changed, the liquid level in the capillary tube rises or falls, the camera takes pictures of the liquid level scale of the capillary tube and transmits the pictures to the computer, the computer reads and identifies the pictures, and the front and back readings of the liquid level of the capillary tube are obtained, so that the change of the liquid level of the capillary tube is monitored, and the change curve of the internal stress of the plating layer along with the time is displayed on the computer after the processing of a software system.
6. The method of operating a device for measuring stresses in a coating according to claim 5, wherein: the camera shoots scales where the liquid level in the capillary is located, the shooting time difference is correspondingly adjusted according to the electroplating speed, the picture is transmitted to the computer, the computer identifies the picture and reads the liquid level scales, and the liquid level variation is monitored through the capillary liquid level scales of adjacent pictures.
7. The method of operating a device for measuring stresses in a coating according to claim 5, wherein: the calculation method of the internal stress of the plating layer comprises the following steps: firstly, a computer identifies a picture transmitted by a camera to read the height variation of the liquid level of the capillary tube, then derivation is carried out based on a Stoney formula, data processing and calculation are carried out through a software system of the computer, and finally the internal stress of a corresponding coating is obtained.
8. The method of operating a device for measuring stresses in a coating according to claim 5, wherein: the computer is used for controlling starting, electrode plate sliding distance, photo transmission and recognition and signal acquisition, and performing data conversion and processing on the electric signals to finally convert the electric signals into stress change curves.
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