CN110470573B - Method for accurately measuring wetting angle of slag interface by using straight thermocouple - Google Patents
Method for accurately measuring wetting angle of slag interface by using straight thermocouple Download PDFInfo
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Abstract
The invention discloses a method for accurately measuring wetting angles of interfaces of molten slag and different coatings by using a straight thermocouple, which is used for researching the interface wetting characteristics of high-temperature molten slag. Most of metallurgical reactions are multi-phase reactions carried out on phase interfaces, the reaction speed is closely related to the size and the properties of the phase interfaces, and the research and calculation of the wettability of slag and the interfaces are particularly important. The method provided by the invention is based on a laboratory high-temperature melting experiment, and combines a monofilament thermocouple technology, so that the problem of how to simply, conveniently, rapidly and accurately measure the wetting angle of the interface between the molten slag and different coatings at high temperature is solved.
Description
Technical Field
The invention discloses a method for accurately measuring interface wettability of molten slag and a coating material, belonging to the technical field of comprehensive utilization of metallurgical slag; relates to a method for characterizing the wettability of metallurgical slag.
Background
The wetting angle is a measure of the wetting properties of the slag on the solid material. When the wetting angle is less than 90 degrees, the wetting property of the slag on the solid is good; when the wetting angle is more than 90 deg., the wetting property of the slag with respect to the solid is poor. In an extreme case, when the wetting angle is 0 degrees, the solid is completely wetted by the slag, and the solid and the slag are not easy to separate; whereas at a wetting angle of 180 deg., the solids are not wetted at all by the slag. Obviously, the smaller the interfacial tension between the slag and the solid material, the smaller the wetting angle, and the better the slag wets the solid. And vice versa.
Metallurgy often encounters situations where the melt is in contact with solid materials, such as contact between metal melt, molten matte, slag or molten salt and furnace lining or electrode materials. Taking aluminum electrolysis as an example, the wettability of the carbon material by the electrolyte has a great influence on the electrolysis process itself and the life of the electrolytic cell. The electrolyte has good wettability, so that the permeation and corrosion of the electrolyte to the lining and the bottom of the electrolytic cell can be accelerated, and the premature damage of the electrolytic cell can be caused; poor wetting property and easy generation of anode effectThis should result in a sharp rise in cell voltage, increased power consumption, etc. Taking continuous casting mold flux as an example, the mold flux has an important function of absorbing inclusions, and researches show that the wetting angle between the TiN inclusions and certain molten steel is 109.8 degrees and the wetting angle between the TiN inclusions and certain mold flux is only 25.6 degrees under the condition of 1550 ℃, which shows that the TiN and the mold flux have good wettability and are beneficial to the mold flux to absorb the TiN inclusions from the molten steel; in addition, studies have shown that certain mold flux is responsible for TiO2And TiN inclusions, which indicates that the same mold flux has different wettability for different inclusions, resulting in different absorption ability for different inclusions. Therefore, the characterization of the wettability of the molten mold flux and different interfaces is very important.
The wetting angle is mainly calculated by using a Young-Dupre equation according to an empirical formula or an established system, but the slag is a complex compound consisting of a plurality of substances, the content is difficult to strictly measure, the wetting property is related to each operating parameter, the wetting angle calculated by using the equation is a numerical value in an ideal state, the wetting angle of the slag under the actual condition is difficult to accurately describe, a large error exists, the reference meaning is not large, and the reliability is low. The slag needs to be melted at high temperature, and the wetting angle needs to be measured at high temperature, which also brings certain operation difficulty.
The subject group has some previous research studies on measuring interfacial wettability of covering slag, for example, the results of the wetting of the covering slag by using the monofilament U-type thermocouple technology are disclosed In "High-Temperature Properties of Mold fluorine assisted and Measured In Situ by simple/Double Hot-thermo-output technique", which is published by Lupeheng 2018 In JOM. Firstly, taking about 50mg of powder covering slag at the arc position of a bare platinum-rhodium wire thermocouple; then, heating the thermocouple to 1500 ℃ at the heating rate of 15 ℃/s to melt the casting powder, wherein the liquid slag has certain expansion, and one part of the liquid slag at the arc position expands to other positions of the thermocouple to form a semi-elliptical liquid bead; and finally, fitting the semi-elliptical liquid bead by using the existing software of the subject group, and obtaining a wetting angle between the liquid slag and the thermocouple so as to represent the interface wettability of the protective slag. Subsequently, the king hucho et al, Chongqing university, also simulates the Method of using a U-shaped single-wire Thermocouple technology to study the wettability of the mold flux in this subject group, and also develops Based on the expansion of the Surface Tension of the molten slag, and discloses the study result in a meeting paper "a Novel Method of Surface Tension Test for Melt slices Based on Hot thermoplastic Technique", published in the TMS meeting in 2019. According to the description, the study method is that the thermocouple temperature is raised to 1500 ℃ and maintained at the temperature under the air atmosphere; melting a sample on the thermocouple to form a semi-elliptical liquid bead, and storing the central axis of the liquid bead to be parallel to the observation surface; then, fitting the shape of the liquid bead by using Image J software and obtaining the size of a wetting angle; and finally, substituting the wetting angle and the interface factor parameters of related substances in the literature into a Young equation to calculate the interfacial tension between the liquid bead and the thermocouple. However, as the research goes further, the method is found to have randomness; and the results of the measurements are not effectively verified and calibrated.
Summary of the invention
On the basis of the original exploration technology, the invention aims to solve the problem that the method has randomness; and the measurement result cannot be effectively verified and calibrated, and the like, so that the method for measuring the interface wettability of the slag and the coating material is provided.
The invention relates to a method for accurately measuring a slag interface wetting angle by using a straight thermocouple, which comprises the following steps: heating a straight type single-wire thermocouple by adopting the straight type single-wire thermocouple, contacting the part A of the straight type single-wire thermocouple with slag to be measured to dip sufficient powder slag, and transversely placing the thermocouple; then heating until the powder slag is melted; after the temperature is kept for 3-5 minutes, due to the existence of interfacial tension of the slag, the slag can form an elliptical liquid bead on the straight thermocouple, the shape of the liquid bead formed by the slag is shot by using high-definition DV, and a slag picture is stored; processing the picture of the intercepted molten slag liquid bead by software to ensure that the fitting curve is tangent with the ellipse of the molten melt liquid bead in the picture; after the fitting is finished, reading a wetting angle formed by melt liquid beads from the parameter dialog box; the part A of the straight monofilament thermocouple is any part except the end part;
defining: dividing the same elliptic liquid bead into an upper liquid bead and a lower liquid bead by taking a straight monofilament thermocouple as a boundary; 4 wetting angles exist on the same slag picture, wherein 2 wetting angles are arranged on the contact surface of the upper end liquid bead and the straight type single-wire thermocouple, and 2 wetting angles are also arranged on the contact surface of the lower end liquid bead and the straight type single-wire thermocouple; comparing the wetting angles on the contact surfaces of the upper end liquid bead and the lower end liquid bead with those of the straight type single-wire thermocouple, and when the error of the obtained wetting angle is more than 5%; judging the obtained result to be an invalid result; and when the error of the obtained wetting angle is less than or equal to 10%, judging that the obtained result is a valid result. The error is calculated in the following way: the maximum value of the wetting angle on the contact surface of the upper end liquid bead and the lower end liquid bead of the same elliptic liquid bead and the straight type single-wire thermocouple is defined as B, and the error is | the wetting angle on the contact surface of the upper end liquid bead and the straight type single-wire thermocouple-the wetting angle on the contact surface of the lower end liquid bead and the straight type single-wire thermocouple, |/B100%.
The invention relates to a method for accurately measuring a slag interface wetting angle by using a straight thermocouple, wherein the straight monofilament thermocouple is a straight platinum-rhodium wire thermocouple or a straight platinum-rhodium wire thermocouple with a coating; the coating is selected from one of a ceramic coating, a metal coating and a ceramic-metal coating, the melting temperature of the coating is higher than that of the slag charge to be measured, and the coating does not melt in the measuring process.
The invention discloses a method for accurately measuring a slag interface wetting angle by using a straight thermocouple, which comprises the steps of heating the straight thermocouple to 600-700 ℃, contacting the part A of the straight thermocouple with slag to be measured, controlling each contact point to stick powder slag with the weight of more than or equal to 5mg and preferably 5-10 mg, and then heating until the powder slag is molten.
Preferably, at least 2 contact points are provided on the straight monofilament thermocouple.
As a further preferred scheme, at least 2 contact points on the straight type monofilament thermocouple have unequal amounts of adhered slag. The slag sample taken at each contact point was not completely spread and was concentrated within 0.5cm of the length of the straight thermocouple.
The invention relates to a method for accurately measuring a slag interface wetting angle by using a straight thermocouple, which heats the straight thermocouple to 600-700 ℃ at a heating rate of 10-20 ℃/s.
The invention relates to a method for accurately measuring a slag interface wetting angle by using a straight thermocouple, which comprises the steps of contacting part A of the straight thermocouple with a slag to be measured to dip sufficient powder slag, and then continuously heating at a heating rate of 5-10 ℃/s until the powder slag is molten.
The invention relates to a method for accurately measuring the interface wetting angle of molten slag by using a straight thermocouple, wherein the atmosphere is controlled in the whole slag melting process and the interface wetting angle forming process; the atmosphere is selected from one of air atmosphere, reducing atmosphere and protective atmosphere, and when the protective atmosphere is adopted, the flow of protective gas is controlled to be 200-300 mL/min. The protective atmosphere is selected from at least one of nitrogen and argon, and the reducing atmosphere is selected from at least one of carbon monoxide and hydrogen.
The invention relates to a method for accurately measuring a wetting angle of a slag interface by using a straight thermocouple, which is characterized in that an intercepted slag liquid bead picture is processed by software, and the operation of enabling a fitting curve to be tangent with an ellipse of a melt liquid bead in the picture is as follows: selecting '16-bit or 8-bit' in an Image-Type mode of the software to adjust the picture into a format which can be processed under the software; then, Li is selected in an Adjust-Auto Threshold-Method mode, so that molten slag liquid beads in the picture are white, and the background is black; calling a wetting angle fitting operation dialog box in the Plugins-Drop-analysis-LB-ADSA function, and adjusting each fitting parameter to ensure that the fitting curve is tangent to the ellipse of the melt liquid bead in the picture; the software is Image J software.
The invention skillfully adopts the straight thermocouple, and solves the problem of randomness in the prior art. Meanwhile, by adopting the technology designed by the invention, a plurality of contact points can be arranged on a straight thermocouple, and the data accuracy is further ensured by analyzing and comparing the data of the plurality of contact points. According to the invention, the slag bonding amount of at least two points is selected to be inconsistent (within a certain range) on a plurality of contact points, so that the slag bonding amount is considered, and a necessary condition is provided for further obtaining accurate data. In addition, the invention can select the coating as a research object, and the coating can simulate the real environment of an industrial construction site, which provides necessary conditions for obtaining more real data. Meanwhile, the direct thermocouple is adopted, so that the method has obvious advantages in the research of the wetting angle of the atmosphere on the interface of the molten slag, and particularly, the data obtained by the method is more objective in the research of the influence of the gas flow rate on the wetting angle.
Compared with the prior exploration method, the invention is improved in the following aspects and has the following advantages: (1) in the aspect of the shape of the formed liquid bead, a large amount of slag (about 50mg) is taken and melted at the arc position of a thermocouple, the liquid bead expands to a straight position to form a plurality of liquid beads due to the expansibility of high-temperature melt, and then the proper liquid bead is selected from pictures for processing; the invention emphasizes that the straight thermocouple is adopted for slag taking, the obtained slag amount range is determined to be 5-10 mg, the influence of the bending of the thermocouple, the insufficient slag amount and other conditions on the formation of the liquid bead shape is ensured, the liquid beads with the same shape are formed on the upper part and the lower part of the thermocouple, the results are reproduced twice in one experiment, the experiment error is comprehensively reduced, and the experiment reliability is improved. (2) The exploration method is mainly carried out in the air atmosphere in the aspect of experimental atmosphere; the method can be carried out under the corresponding atmosphere according to the actual working condition. In addition, when the influence of the gas flow rate on the experimental result is researched, the method is more objective (3) in the aspect of researching the wettability of the slag and different interfaces, and the wettability of the slag and different interfaces in the actual process is compared by mainly researching the wettability of the interface between the slag and the platinum-rhodium wire; the invention newly designs a layer of coating material to be plated on the thermocouple, slag is melted but the coating material is not melted by heating the thermocouple, so that a three-phase interface of slag-air-coating material (liquid-gas-solid) is formed, and the interface wettability of the slag and the specific material in the actual working condition is simulated really instead of being simulated by the interface wettability of the slag and the platinum-rhodium wire.
The improvement of the exploration method of the invention ensures that the method of the invention has good reliability and reproducibility and can simulate the actual working condition more truly.
Drawings
FIG. 1 is a graph of the wetting angle topography of experimental slag of example 1;
FIG. 2 is a graph of the wetting angle topography of the experimental slag of example 2;
FIG. 3 is a graph of the wetting angle topography of the experimental slag of example 3;
FIG. 4 is a graph of the wetting angle topography of experimental slag of comparative example 1;
FIG. 5 is a graph of the wetting angle topography of experimental slag of comparative example 2.
The specific implementation mode is as follows:
the invention is further illustrated by the following examples, which are intended to be illustrative only and are not intended to be in any way limiting.
In the embodiment of the invention, the slag sample on each contact point cannot be completely spread and needs to be concentrated in the range of 0.5cm of the straight thermocouple.
Example 1
The experimental procedure of this example was to first grind the test slag sample (through a 100 mesh screen) and plate a layer of TiO on a platinum rhodium wire thermocouple2Coating; then, the temperature of the platinum-rhodium wire is raised to 700 ℃ at the heating rate of 10 ℃/s, enough slag samples (5 mg, 8mg and 10mg in sequence) are respectively dipped at 3 positions, and then argon with the flow rate of 300mL/min is introduced for atmosphere protection; then, the temperature of the thermocouple attached with the slag sample is continuously increased to 1500 ℃ at the temperature increasing rate of 10 ℃/s to melt the slag sample and the temperature is kept for 3 minutes. The shape of the liquid slag is shot after the liquid slag forms a stable liquid bead on the thermocouple, and the liquid slag and TiO are obtained by software fitting2Wetting angle between the coatings, the results for the 8mg sample point are shown in FIG. 1. From the fitting results in the figures, the wetting angle formed by the upper end bead is 44.791 °, the wetting angle formed by the lower end bead is 44.682 °, and the error is only 0.24%. Fitting the data of 5mg sampling points and 10mg sampling points at the same time, and finding that the error between the wetting angle formed by the liquid beads at the upper ends of the 5mg sampling points and the wetting angle formed by the liquid beads at the upper ends of the 8mg sampling points is less than 3 percent; the wetting angle error formed by the liquid beads at the lower end is less than 4 percent.
Example 2
In the experimental process of the example, the test slag sample is firstly ground into powder (screened by a 100-mesh screen), and a TiN coating is plated on the platinum rhodium wire thermocouple; heating the thermocouple to 700 ℃ at a heating rate of 15 ℃/s to pick up enough slag sample (8 mg); then, the temperature of the thermocouple attached with the slag sample is increased to 1450 ℃ at the temperature increasing rate of 8 ℃/s in the direct air atmosphere to melt the slag sample and the temperature is kept for 4 minutes. The shape of the liquid slag after forming a stable liquid bead on the thermocouple is photographed, and the wetting angle of the liquid slag and the TiN coating is obtained by software fitting, and the result is shown in the attached figure 2. From the fitting results in the figures, the wetting angle formed by the upper end bead was 45.493 °, the wetting angle formed by the lower end bead was 45.415 °, and the error was only 0.17%.
Example 3
In the experimental process of the embodiment, the test slag sample is firstly ground into powder (screened by a 100-mesh screen), then the temperature of a bare platinum-rhodium wire thermocouple is increased to 600 ℃ at the heating rate of 20 ℃/s to pick up enough slag sample (8mg), and then nitrogen with the flow rate of 200mL/min is introduced for atmosphere protection; then, the thermocouple temperature with the slag sample is continuously increased to 1400 ℃ at the temperature increasing rate of 5 ℃/s to melt the slag sample and the temperature is kept for 5 minutes. The shape of the liquid slag after forming a stable liquid bead on the thermocouple is photographed, and the wetting angle between the liquid slag and the platinum-rhodium wire is obtained by software fitting, and the result is shown in figure 3. From the fitting results in the figures, the wetting angle formed by the upper end bead is 46.466 °, the wetting angle formed by the lower end bead is 46.258 °, and the error is only 0.45%.
Comparative example 1
The experimental process of the comparative example is that the test slag sample is firstly ground into powder (screened by a 100-mesh screen); plating TiO on the substrate at a heating rate of 20 ℃/s2Heating a U-shaped platinum rhodium wire thermocouple of the coating to 700 ℃ to dip enough slag samples (the thermocouple has certain curvature), and then introducing argon with the flow of 300mL/min for atmosphere protection; then, the temperature of the thermocouple attached with the slag sample is continuously increased to 1500 ℃ at the temperature increasing rate of 15 ℃/s to melt the slag sample and the temperature is kept for 3 minutes. The shape of the liquid slag is shot after the liquid slag forms a stable liquid bead on the thermocouple, and the liquid slag and TiO are obtained by software fitting2Method for producing a coatingThe wetting angle therebetween, the results are shown in fig. 4. As can be seen from the figure, the thermocouple is slightly bent downwards, so that the shapes of liquid beads at the upper end and the lower end of the thermocouple are inconsistent; from the fitting results, the wetting angle of the upper bead was 47.079 °, the wetting angle of the lower bead was only 39.385 °, and the experimental error was 16.34%.
Comparative example 2
The experimental process of the comparative example is that the test slag sample is firstly ground into powder (screened by a 100-mesh screen), then the temperature of the bare platinum-rhodium wire thermocouple is increased to 500 ℃ at the temperature rising rate of 5 ℃/s to dip the slag sample (because the sintering temperature is not enough, the enough slag quantity cannot be dipped), and then nitrogen with the flow rate of 200mL/min is introduced for atmosphere protection; then, the temperature of the thermocouple attached with the slag sample is continuously increased to 1450 ℃ at the temperature increasing rate of 5 ℃/s to melt the slag sample and keep the temperature for 5 minutes. The shape of the liquid slag after forming a stable liquid bead on the thermocouple is photographed, and the wetting angle between the liquid slag and the platinum-rhodium wire is obtained by software fitting, and the result is shown in figure 5. As can be seen from the figure, the liquid bead at the upper end of the thermocouple is full in shape, the liquid bead at the lower end of the thermocouple is flat, and the middle of the thermocouple is exposed, which indicates that the sample quantity is not enough; from the fitting results, the wetting angle of the upper bead was 50.813 °, the wetting angle of the lower bead was 32.326 °, and the experimental error was 36.38%.
Claims (7)
1. A method for accurately measuring the wetting angle of a slag interface by using a straight thermocouple is characterized by comprising the following steps: heating a straight type single-wire thermocouple by adopting the straight type single-wire thermocouple, contacting the part A of the straight type single-wire thermocouple with slag to be measured to dip sufficient powder slag, and transversely placing the thermocouple; then heating until the powder slag is melted; after the temperature is kept for 3-5 minutes, due to the existence of interfacial tension of the slag, the slag can form an elliptical liquid bead on the straight thermocouple, the shape of the liquid bead formed by the slag is shot by using high-definition DV, and a slag picture is stored; processing the picture of the intercepted molten slag liquid bead by software to ensure that the fitting curve is tangent with the ellipse of the molten melt liquid bead in the picture; after the fitting is finished, reading a wetting angle formed by melt liquid beads from the parameter dialog box; the part A of the straight monofilament thermocouple is any part except the end part; at least 2 contact points are arranged on the straight type single-wire thermocouple; at least 2 contact points on the straight monofilament thermocouple have unequal amounts of slag adhered; the slag sample on each contact point can not be completely spread and needs to be concentrated in the range of 0.5cm of the straight thermocouple;
defining: dividing the same elliptic liquid bead into an upper liquid bead and a lower liquid bead by taking a straight monofilament thermocouple as a boundary; 4 wetting angles exist on the same slag picture, wherein 2 wetting angles are arranged on the contact surface of the upper end liquid bead and the straight type single-wire thermocouple, and 2 wetting angles are also arranged on the contact surface of the lower end liquid bead and the straight type single-wire thermocouple; comparing wetting angles on contact surfaces of the upper end liquid bead and the lower end liquid bead with those of the straight type single-wire thermocouple, and when the deviation of the obtained wetting angles is more than 5%; judging the obtained result to be an invalid result; when the deviation of the wetting angle is not more than 5%, the obtained result is judged to be a valid result.
2. The method for accurately measuring the wetting angle of the slag interface by using the straight thermocouple as claimed in claim 1, wherein: the straight type single-wire thermocouple is a straight type platinum rhodium wire thermocouple or a straight type platinum rhodium wire thermocouple with a coating; the coating is selected from one of a ceramic coating, a metal coating and a ceramic-metal coating, the melting temperature of the coating is higher than that of the slag charge to be measured, and the coating does not melt in the measuring process.
3. The method for accurately measuring the wetting angle of the slag interface by using the straight thermocouple as claimed in claim 1, wherein: heating the straight type single-wire thermocouple to 600-700 ℃, contacting the part A of the straight type single-wire thermocouple with the slag to be measured, controlling each contact point to stick powder slag of which the quantity is more than or equal to 5mg, and then heating until the powder slag is molten.
4. A method for accurately measuring the wetting angle of the slag interface with a straight thermocouple according to claim 3, wherein: the straight type single-wire thermocouple is heated to 600-700 ℃ at the heating rate of 10-20 ℃/s.
5. The method for accurately measuring the wetting angle of the slag interface by using the straight thermocouple as claimed in claim 1, wherein: and contacting the part A of the straight type single-wire thermocouple with slag to be measured to pick up sufficient powder slag, and then continuously heating at the heating rate of 5-10 ℃/s until the powder slag is molten.
6. The method for accurately measuring the wetting angle of the slag interface by using the straight thermocouple as claimed in claim 1, wherein: controlling atmosphere in the whole slag melting process and the interface wetting angle forming process; the atmosphere is selected from one of air atmosphere and protective atmosphere, and when the protective atmosphere is adopted, the flow of protective gas is controlled to be 200-300 mL/min.
7. The method for accurately measuring the wetting angle of the slag interface by using the straight thermocouple as claimed in claim 1, wherein:
processing the picture by the intercepted slag liquid bead picture through software, and enabling the fitting curve to be tangent with the ellipse of the melt liquid bead in the picture as follows: selecting '16-bit or 8-bit' in an Image-Type mode of the software to adjust the picture into a format which can be processed under the software; then, Li is selected in an Adjust-Auto Threshold-Method mode, so that molten slag liquid beads in the picture are white, and the background is black; calling a wetting angle fitting operation dialog box in the Plugins-Drop-analysis-LB-ADSA function, and adjusting each fitting parameter to ensure that the fitting curve is tangent to the ellipse of the melt liquid bead in the picture; the software is Image J Image processing software.
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| CN102393350A (en) * | 2011-09-28 | 2012-03-28 | 淮阴工学院 | Method for measuring wetting angle between titanium alloy melt and oxide ceramic |
| CN104407007A (en) * | 2014-12-16 | 2015-03-11 | 中南大学 | Method for determining melting temperature interval and melting behavior of metallurgical slag |
| CN109655381A (en) * | 2019-01-04 | 2019-04-19 | 江苏理工学院 | A kind of measurement method of high temperature aluminum/aluminium alloy drop angle of wetting |
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