CN112748108A - Real-time measuring system for wettability parameter of space high-temperature melt material - Google Patents
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Abstract
The invention discloses a real-time measuring system for wettability parameters of a space high-temperature melt material, which comprises the following components: the device comprises a substrate, a high-temperature furnace, a vacuum pumping system, a laser light source, a high-resolution camera and an image processing system; the substrate is arranged in a hearth of the high-temperature furnace and used for placing a solid metal sample; the high-temperature furnace is used for preventing the surface of the metal sample from being oxidized and denatured by utilizing a high-vacuum environment; heating the solid metal sample to a high temperature state, and wetting the metal sample with the graphite substrate after the metal sample is completely melted; the vacuum air extraction system is used for performing vacuum air extraction on the hearth of the high-temperature furnace to enable the hearth of the high-temperature furnace to reach a set vacuum environment; the laser light source is used for providing illumination for the interior of the hearth of the high-temperature furnace; the high-resolution camera is used for collecting an image of the molten metal sample and sending the image to the image processing module; the image processing system is used for measuring wettability parameters including contact angles and surface tension of the high-temperature metal sample on the solid substrate in real time through an image analysis method and storing the wettability parameters.
Description
Technical Field
The invention relates to the field of space materials, in particular to a real-time measuring system for wettability parameters of a space high-temperature melt material.
Background
The ability or tendency of a liquid to spread across a solid surface is known as wettability. Wetting generally refers to the process of a liquid (e.g., water droplets, metal droplets, etc.) displacing a fluid (usually a gas, but also other liquids) at a solid interface.
The wetting angle is commonly used by scholars to discuss the wettability between liquid-solid interfaces. The definition of the contact angle is: the three-phase equilibrium point of s (solid phase), l (liquid phase) and g (gas phase) is used as the included angle between the tangent of the liquid-gas interface and the liquid-solid interface. In the beginning of the nineteenth century, Thomas Young analyzes the wetting process by using mechanical knowledge, establishes a physical property model to describe the balance relation of interfacial energy of an interface generated among solid, liquid and gas phases when liquid is balanced on a solid substrate, and deduces a famous Young's equation:
cosθ＝(σgs-σls)/σgl
wherein σgsRepresents the interfacial tension between the solid and gas phases, σlsRepresents the interfacial tension between the liquid and solid phases, σglRepresents the interfacial tension between the gas and liquid phases and theta represents the contact angle of the liquid-solid interface. The contact angle is usually studied by several methods, including angulometry, force measurement, length measurement, transmission and digital image analysis, among which the most effective and widely used method is digital image analysis.
The wetting behavior and the interface interaction between the liquid and the solid phases are common physical and chemical phenomena in the material preparation and processing processes, and play a key role in the preparation and processing processes of many materials such as alloy smelting, welding, composite material preparation, 3D printing and the like, so the research on the wetting behavior of the high-temperature melt also influences the research on the material science to a great extent. However, the gravity environment has a significant influence on the phenomenon, and the relevant data measured in the ground environment can be deviated due to the influence of gravity, so that the contact angle of the sample can be studied in the space under the microgravity condition to obtain a more accurate measurement result.
The life expectancy of a space station operating in space is generally more than ten years, space components are affected by temperature fatigue, ion radiation, space particle or space debris impact, impact during butt joint and the like during space operation, and on-orbit maintenance is a necessary means for realizing long service life, high reliability and high safety of the manned spacecraft. Welding is one of the important means for on-track maintenance. The wetting behavior and interfacial reaction between materials are one of the key scientific issues that need to be addressed for space welding. In addition, it is one of the key factors that determine the quality of the outer space additive manufactured product. With the establishment of Chinese space stations, more and more space material science experiments can be performed to study the measurement of the wettability of the molten metal drops under microgravity in space. If the high-temperature wettability of the metal is analyzed by a digital image analysis method, the method is greatly limited due to the limitations of space station experiment resources and conditions (including data storage resources, data transmission resources, time resources, astronauts' operation resources and the like).
For measuring the wettability of high-temperature melts, obtaining accurate wettability measurements using commercially available measuring instruments presents certain difficulties, mainly due to the following:
1. the gravity environment has obvious influence on the wetting phenomenon, and the related data measured in the ground environment can be deviated due to the influence of gravity.
2. The analysis of the high-temperature wettability of the metal by a digital image analysis method is limited by experimental resources and conditions of a space station.
3. Usually, the melting point of the space material is above 1000 ℃, and the highest measuring temperature of a measuring instrument for wettability commonly used in the market is below 300 ℃, so that the requirement cannot be met.
Therefore, the experimental system capable of monitoring the wettability of the liquid drops of the high-temperature metal melt in real time, effectively acquiring experimental images, processing the images in real time and obtaining the wettability parameters of the liquid drops of the metal melt is developed, and the experimental system has important significance for developing the wettability research of the liquid drops of the metal melt under the space microgravity.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a real-time measuring system for wettability parameters of a space high-temperature melt, which comprises: the device comprises a substrate, a high-temperature furnace, a vacuum pumping system, a laser light source, a high-resolution camera and an image processing system;
the substrate is arranged in a hearth of the high-temperature furnace and used for placing a solid metal sample;
the high-temperature furnace is used for preventing the surface of the metal sample from being oxidized and denatured by utilizing a high-vacuum environment; heating the solid metal sample to a high temperature state, and wetting the metal sample with the graphite substrate after the metal sample is completely melted;
the vacuum air extraction system is used for performing vacuum air extraction on the hearth of the high-temperature furnace to enable the hearth of the high-temperature furnace to reach a set vacuum environment;
the laser light source is used for providing illumination for the interior of a hearth of the high-temperature furnace;
the high-resolution camera is used for collecting an image of the molten metal sample and sending the image to the image processing module;
the image processing system is used for measuring wettability parameters including contact angles and surface tension of the high-temperature metal sample on the solid substrate in real time through an image analysis method and storing the wettability parameters.
As an improvement of the system, the high-temperature furnace adopts a double-layer cylinder structure, and the hearth material is made of high-purity alumina; the maximum working temperature can reach 1700 ℃.
As an improvement of the above system, the substrate is made of a metal material which does not react at a high temperature.
As an improvement of the above system, the vacuum pumping system comprises a mechanical pump and a molecular pump, and the vacuum degree which can be achieved by using the mechanical pump is 10-2Torr, the degree of vacuum which can be achieved using a molecular pump is 10-5Torr。
As an improvement of the above system, the vacuum degree of the vacuum environment is less than 5 x 10-5Torr。
As an improvement of the system, the high-resolution camera is a gray scale camera using a CCD chip, the resolution is 2048 × 2048 or more, and the shooting frequency can reach 26fps or more.
As an improvement of the system, the laser light source adopts a laser emitter with adjustable light intensity.
As an improvement of the above system, the image processing system is implemented by the following steps:
(1) judging the melting state of the metal melt based on a perceptual hash algorithm, and effectively collecting an experimental image of the metal melt; judging the image by using the algorithm, increasing the sampling rate of the image when the sample begins to melt, and sampling at a lower sampling rate before the sample is melted;
(2) preprocessing the collected metal melt image by adopting an Otsu Law method or a Canny operator to obtain the outline of the metal melt;
(3) calculating the surface tension of the metal melt in real time by adopting Young-Laplace contour fitting, and calculating the contact angle of the metal melt by adopting Young-Laplace contour fitting, ellipse fitting, exponential fitting or polynomial fitting;
(4) the wettability parameters surface tension and contact angle are stored.
The invention has the advantages that:
the system of the invention utilizes the space microgravity environment to reduce the influence of gravity on the measurement of the wettability parameter; the surface of the metal melt is prevented from being oxidized and denatured by using a high vacuum environment; a high-temperature furnace is used for completing heating and temperature control, and the requirement of a high-temperature melt wettability experiment is met; judging the molten state of the metal melt based on a perceptual hash algorithm to realize effective acquisition of wettability experiment images; the contact angle, surface tension and other wettability parameters of the metal melt on the substrate were measured by digital image analysis and the programmed QT program.
Drawings
FIG. 1 is a block diagram of a real-time measurement system for wettability parameters of a spatial high-temperature melt material according to the present invention;
FIG. 2 is a schematic view of a high heat furnace and its built-in substrate according to the present invention;
fig. 3 is a block diagram of the high heat furnace composition of the present invention.
Detailed Description
The invention discloses a real-time measuring system for wettability parameters of a space high-temperature melt material, which comprises: high temperature furnace, vacuum pumping system, laser light source, high resolution camera and image processing system. Preventing the surface of the metal sample from being oxidized and denatured by using a high vacuum environment; heating a metal sample to be measured on a solid substrate by using a high-temperature furnace to meet the requirement of measuring the wettability of the high-temperature melt; the shooting rate of the camera can be automatically adjusted through image processing software, and intelligent and effective collection of wettability experiment image data is realized; and measuring and storing wettability parameters of the high-temperature metal sample on the solid substrate including a contact angle and surface tension in real time by adopting an image analysis method and image processing software compiled by Qt. The invention provides a method for rapidly, economically and effectively solving the problem of measuring the wettability of a space high-temperature melt material and the surface of a substrate, provides accurate parameter input for the simulation calculation of future materials, and provides technical support and experimental data accumulation for the scientific research of space stations and space materials in the future.
As shown in FIG. 1, the present invention provides a real-time measurement system for wettability parameter of a spatial high-temperature melt material, comprising: graphite substrate, high temperature furnace, vacuum pumping system, laser light source, high resolution camera and image processing system. Preventing the surface of the metal sample from being oxidized and denatured by using a high vacuum environment; heating a metal sample to be measured on a solid substrate by using a high-temperature furnace to meet the requirement of measuring the wettability of the high-temperature melt; the shooting rate of the camera can be automatically adjusted through image processing software, and intelligent and effective collection of wettability experiment image data is realized; and measuring and storing wettability parameters of the high-temperature metal sample on the solid substrate including a contact angle and surface tension in real time by adopting an image analysis method and image processing software compiled by Qt.
As shown in fig. 2, the high temperature furnace is a measuring chamber for measuring the wettability of the high temperature metal melt, the furnace chamber is a cylinder with a high purity alumina material and a double-layer shell structure, and the graphite substrate is arranged in the furnace chamber. During the experiment, a metal sample is placed on a graphite substrate, is heated by a high-temperature furnace and is melted into a liquid state, and is wetted with the graphite substrate. The high-temperature furnace is also provided with a temperature control module, the temperature is controlled by adopting a PID control mode, and the temperature control precision can reach +/-1 ℃. As shown in the structure diagram of the temperature control module shown in fig. 3, the temperature control module includes a temperature sensor, a temperature thermocouple, a temperature controller and a power regulator, and the temperature sensor sends the collected temperature in the high-temperature furnace hearth to the temperature controller after acquiring the temperature in the high-temperature furnace hearth by the temperature thermocouple; the temperature controller sends a temperature control instruction to the power regulator, the high-temperature furnace is controlled to work according to the temperature control instruction, the temperature in the hearth can be controlled to be the temperature required by melting of the metal sample, and the metal sample is wetted with the graphite substrate after being completely melted.
The vacuum pumping system comprises a mechanical pump and a molecular pump and is used for vacuum pumping of the high-temperature furnace hearth. A required vacuum environment is obtained through a vacuum pumping system, and the test of the high-temperature metal melt material wettability experiment requires that the vacuum degree is less than 5 multiplied by 10 < -2 > Torr, so that the surface oxidation of the high-temperature melt is avoided, and the accuracy of the measurement result is not influenced.
The laser light source adopts a laser emitter with adjustable light intensity to polish the hearth of the high-temperature furnace. Due to the internal structure of the high-temperature furnace hearth, a high-resolution camera can obtain a clear experimental image of the high-temperature metal melt wettability experiment under the lighting of a laser light source.
The high-resolution camera adopts a gray camera, the acquisition rate is more than 26 frames/second, the acquired image resolution is 2048 × 2048, and the high-resolution camera is connected to the computer through a USB interface and is used for acquiring the wetting images of the metal melt and the graphite substrate in the wettability experiment.
The image processing system is software for measuring various wettability parameters in a wettability experiment, is written by QT, and can detect that a sample starts to melt in real time and acquire wettability experiment images; processing the collected image, obtaining a fitting curve of the high-temperature metal melt after operations such as pretreatment, edge contour extraction, contour fitting and the like, and calculating various wettability parameters including contact angles and surface tension of the sample through the fitting curve; in addition, the wettability measurement software also has the functions of off-line processing and batch processing, and can efficiently process the existing pictures and calculate the wettability parameters.
The specific implementation process comprises the following steps:
(1) judging the melting state of the metal melt based on a perceptual hash algorithm, and effectively collecting an experimental image of the metal melt; the image is judged by the algorithm, the sampling rate of the image is increased when the sample begins to melt, and the sampling is carried out at a lower sampling rate before the sample melts. This can save the storage space of the image greatly (only 10% of the traditional method is needed), and at the same time, the transmission quantity of the image is greatly reduced.
(2) Preprocessing the collected metal melt image by adopting an Otsu Daohu method and a Canny operator to obtain the profile of the metal melt, calculating wettability parameters including a contact angle and surface tension of the metal melt in real time by using a Young-Laplace profile fitting method, and storing the wettability parameters.
(3) And respectively adopting ellipse fitting, exponential fitting and polynomial fitting methods to calculate the contact angle of the sample, and selecting the most appropriate method for calculation.
The specific measurement process of the invention is as follows:
1. firstly, a software-controlled camera is used for monitoring an experimental process in real time, and a perceptual hash algorithm is used for calculating a perceptual characteristic value of an experimental image in real time; when the experimental sample begins to melt, the perception characteristic value of the experimental image is greatly changed, and the perception characteristic values of the experimental images of adjacent frames or a certain time interval are compared to obtain a perception distance; once the perception distance exceeds the perception threshold, it indicates that the morphology of the sample is changing greatly at this time, the sample is already in a molten state, and the software begins to save the experimental image.
2. The software carries out real-time processing on the stored experimental images: the method comprises binarization based on an Otsu algorithm and edge contour extraction based on a Canny operator, and extraction of the contour of the experimental sample is completed.
3. After contour data of an experimental sample is obtained, fitting processing needs to be carried out on a contour, and a contour fitting method based on a classical Young-Laplace equation of physics is used for measurement software, and Young-Laplace fitting is called Young-Laplace fitting for short. The calculation process of Young-Laplace fitting is as follows:
(1) contact angle
By fitting the coordinates of the points of the curve, the software, according to the definition of the contact angle: making a solid (graphite substrate), liquid (metal molten drop) and gas three-phase contact point as a liquid-gas interface to obtain a tangent line and a liquid-solid interface to obtain an included angle, and obtaining a contact angle between the metal molten drop and the graphite substrate;
(2) radius of contact surface, height of droplet
Two-point coordinates (x) of the metal molten drop contacting the graphite substrate are searched in a fitting curve through software1,y1),(x2,y2) And droplet maximum point coordinate (x)h，yh) Then the contact surface radius R ═ x2-x1L/2, droplet height h ═ yh-(y1+y2)/2；
(3) Volume of
The surface area is determined by considering the sample as a plurality of small circular truncated cones
siRepresenting the side area of the ith small circular truncated cone, and finally calculating:
S＝πRl+πrl
wherein R is the radius of the upper base, R is the radius of the contact surface,
(4) volume of
Similarly to when calculating the surface area, the sample is also considered as a plurality of small circular truncated cones, then the volume
viRepresenting the volume of the ith truncated cone, and finally obtaining V ═ pi h (R)2+r2+Rr)/3；
(5) Surface tension
The formula for calculating the surface tension is γ ═ (Δ ρ) gR'2And/beta, wherein Δ ρ represents the density difference between the droplet and the substrate, g represents the gravitational acceleration, and R' and β are the optimal values obtained after Young-Laplace fitting.
(6) The contact angle may also be calculated using ellipse fitting, exponential fitting, polynomial fitting, and the like.
In the invention:
firstly, preparation before experiment:
firstly, placing a graphite substrate and an experimental sample in a high-temperature furnace hearth, checking a camera shot picture by using measurement software, and adjusting the focal length of a laser light source and a camera to enable a camera shot image to be clear; adjusting the graphite substrate and the experimental sample to be horizontal by using a correction function of the measurement software; finally, some known parameters (such as gravity acceleration, density difference of the melt and the graphite substrate and the like) are pre-input into the measurement software and are used for calculating the wettability parameter.
Secondly, realizing a high vacuum environment:
the method comprises the steps of firstly carrying out normal-temperature air extraction and leakage detection on a high-temperature furnace hearth, and then carrying out vacuum air extraction on the high-temperature furnace hearth by using a mechanical pump and a dry pump. The vacuum degree of the hearth of the high-temperature furnace reaches 5 multiplied by 10 < -2 > Torr through vacuum pumping, and the requirement of a measuring system on high vacuum is realized.
Thirdly, heating the high-temperature furnace:
setting the temperature of the high-temperature furnace by using a temperature control module of the high-temperature furnace, and finally reaching the temperature 100 ℃ higher than the melting point of the experimental sample and preserving the heat for 30 minutes; in the process, the experimental sample is completely melted, and the measuring software controls the camera to intelligently and effectively acquire the experimental image and calculate the wettability parameter in real time.
Fourthly, preserving the wettability parameter:
in the experimental process, the measurement software completes the real-time calculation of the wettability parameter, and the CSV file is used for storing the calculation result of the wettability parameter.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and are not limited. Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (8)
1. A system for real-time measurement of wettability parameters of a spatial high-temperature melt material, the system comprising: the device comprises a substrate, a high-temperature furnace, a vacuum pumping system, a laser light source, a high-resolution camera and an image processing system;
the substrate is arranged in a hearth of the high-temperature furnace and used for placing a solid metal sample;
the high-temperature furnace is used for preventing the surface of the metal sample from being oxidized and denatured by utilizing a high-vacuum environment; heating the solid metal sample to a high temperature state, and wetting the metal sample with the graphite substrate after the metal sample is completely melted;
the vacuum air extraction system is used for performing vacuum air extraction on the hearth of the high-temperature furnace to enable the hearth of the high-temperature furnace to reach a set vacuum environment;
the laser light source is used for providing illumination for the interior of a hearth of the high-temperature furnace;
the high-resolution camera is used for collecting an image of the molten metal sample and sending the image to the image processing module;
the image processing system is used for measuring wettability parameters including contact angles and surface tension of the high-temperature metal sample on the solid substrate in real time through an image analysis method and storing the wettability parameters.
2. The system for measuring the wettability parameter of the spatial high-temperature melt material in real time according to claim 1, wherein the high-temperature furnace has a double-layer cylinder structure, and the hearth of the high-temperature furnace is made of high-purity alumina; the maximum working temperature can reach 1700 ℃.
3. The system for real-time measurement of wettability parameter of a spatial hot-melt material according to claim 2, wherein said substrate is made of a metallic material which does not react at high temperature.
4. The system for real-time measurement of wettability parameter of spatial hot melt material according to claim 1, wherein said vacuum pumping system comprises a mechanical pump and a molecular pump, and the vacuum degree that can be achieved by using said mechanical pump is 10-2Torr, the degree of vacuum which can be achieved using a molecular pump is 10-5Torr。
5. The system for real-time measurement of wettability parameter of spatial hot-melt material according to claim 4, wherein the vacuum degree of said vacuum environment is less than 5 x 10-5Torr。
6. The system for measuring the wettability parameter of the spatial high-temperature melt material in real time according to claim 1, wherein the high-resolution camera is a grayscale camera using a CCD chip, the resolution is 2048 × 2048 or more, and the shooting frequency can reach 26fps or more.
7. The system for measuring the wettability parameter of the spatial high-temperature melt material in real time according to claim 1, wherein the laser light source adopts a laser emitter with adjustable light intensity.
8. The system for measuring the wettability parameter of the spatial high-temperature melt material in real time according to claim 1, wherein the image processing system is implemented by the following steps:
(1) judging the melting state of the metal melt based on a perceptual hash algorithm, and effectively collecting an experimental image of the metal melt; judging the image by using the algorithm, increasing the sampling rate of the image when the sample begins to melt, and sampling at a lower sampling rate before the sample is melted;
(2) preprocessing the collected metal melt image by adopting an Otsu Law method or a Canny operator to obtain the outline of the metal melt;
(3) calculating the surface tension of the metal melt in real time by adopting Young-Laplace contour fitting, and calculating the contact angle of the metal melt by adopting Young-Laplace contour fitting, ellipse fitting, exponential fitting or polynomial fitting;
(4) the wettability parameters surface tension and contact angle are stored.
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| CN113866052B (en) * | 2021-11-23 | 2023-06-23 | 西北大学 | Method for rapidly judging whether wettability of glass powder and silicon substrate is good or bad |
| CN114459959A (en) * | 2021-12-30 | 2022-05-10 | 北京工业大学 | Device and method for measuring high-temperature contact angle of material surface |
| CN114459959B (en) * | 2021-12-30 | 2023-12-08 | 北京工业大学 | Device and method for measuring high-temperature contact angle of material surface |
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