CN113030166A - Measuring device for semi-solid rheological behavior of high-entropy alloy and using method thereof - Google Patents
Measuring device for semi-solid rheological behavior of high-entropy alloy and using method thereof Download PDFInfo
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Abstract
A measuring device for high-entropy alloy semi-solid rheological behavior and a using method thereof relate to a measuring device for alloy semi-solid rheological behavior and a using method thereof. The invention aims to solve the technical problem that the conventional rheological measurement device and method are not directed at high-entropy alloy. The high-entropy alloy rheological behavior measuring device provided by the invention adopts a vacuum chamber design idea, fully considers the technical problem that the high-entropy alloy is easy to oxidize in a semi-solid state, and can fully avoid adverse effects on experiments caused by oxidation by utilizing the vacuum chamber design rheological experimental measurement; the high-entropy alloy rheological behavior measuring device provided by the invention adopts the hydraulic servo transmission mechanism to provide experimental load application, so that the applied displacement precision and load precision can be effectively controlled, and the precision of a high-entropy alloy rheological experiment is ensured.
Description
Technical Field
The invention relates to a device for measuring alloy semi-solid rheological behavior and a using method thereof.
Background
The semi-solid processing technology is a precise near-net forming technology for metal material, and is characterized by that it utilizes the metal semi-solid slurry with spherical crystal solid phase and liquid phase mixed to form high-performance metal component with complex shape under the action of pressure. Due to the laminar filling characteristic of the semi-solid slurry, the semi-solid forming technology is widely applied to the fields of automobiles, motorcycles and 3C, and particularly, with the rapid development of 5G communication in recent years, the semi-solid processing technology shows certain superiority in the aspect of communication heat dissipation shells.
At present, the semi-solid processing technology is mainly applied to aluminum alloy and magnesium alloy materials. Semi-solid processing theory and techniques of other materials are relatively less studied than aluminum and magnesium alloys. However, from the theory of semi-solid processing, all materials having a solid-liquid temperature range are suitable for semi-solid processing. That is, high melting point alloys such as alloy steels, carbon steels, cast irons, copper alloys, titanium alloys, and superalloys may also be semi-solid processed by rheological or thixotropic filling of the semi-solid slurry to form the particular part. The high-entropy alloy is a brand-new solid solution type alloy formed by mixing more than five metal components with equal atomic ratio or near equal atomic ratio. In recent decades, a great deal of research shows that the high-entropy alloy has the characteristics of high strength, high toughness, high hardness, excellent thermal stability and good oxidation resistance and corrosion resistance. Therefore, the high-entropy alloy becomes a novel metal material based on a brand-new alloy design concept and excellent performance. Some high entropy alloys also have a solid-liquid temperature range, i.e., a semi-solid temperature range. Therefore, it also has a possibility of performing semi-solid processing in theory.
The technical advantage of semi-solid processing of metal materials is the special rheological behavior-shear thinning behavior of semi-solid slurries. Therefore, how to study the rheological behavior of the metal material semisolid slurry is a very important research direction in the technical field of semisolid processing. In the process of researching the semi-solid rheological behavior of the metal, the adopted semi-solid slurry rheological measurement device and method are very critical. Based on casting rheology devices and measurement methods, some methods for measuring the rheology of semi-solid slurry are researched and proposed in the semi-solid processing academic and business circles at home and abroad, and special rheology measurement devices are designed and manufactured. However, the current rheological measurement device and method are designed and developed for rheological measurement of low melting point semi-solid slurry of aluminum alloy and magnesium alloy. The rheological measurement method and device for the high-melting-point alloy semi-solid slurry, in particular the high-entropy alloy semi-solid slurry, are not mentioned at home and abroad. The research on the semi-solid processing technology of the high-entropy alloy is also a brand-new scientific research direction, only two students at home and abroad develop some exploratory work in the direction at present, and the research on the semi-solid processing technology of the high-entropy alloy is proved to be feasible. Therefore, in order to promote the research of the high-entropy alloy semi-solid processing technology, an apparatus and a method suitable for rheological behavior measurement of the high-entropy alloy semi-solid slurry must be designed and developed.
Disclosure of Invention
The invention provides a device for measuring semi-solid rheological behavior of a high-entropy alloy and a using method thereof, aiming at solving the technical problem that the conventional rheological measuring device and method do not aim at the high-entropy alloy.
The device for measuring the semi-solid rheological behavior of the high-entropy alloy consists of a vacuum chamber 1, a fixed pressure head 2, a resistance heating unit 4, a movable pressure head 5, a displacement sensor 6, a hydraulic servo transmission device 7, a first thermocouple 8, a second thermocouple 9, a third thermocouple 10, a temperature control device 11, a pressure sensor 12, a vacuumizing device 13, a first heat insulation pad 14, a first graphite gasket 15, a second graphite gasket 16, a second heat insulation pad 17, a first supporting rod 18, a second supporting rod 19, a supporting leg 20, a hinge 21 and a controller;
the vacuum chamber 1 is communicated with an air exhaust port of a vacuum device 13, and the vacuum device 13 is arranged outside the vacuum chamber 1; one end of the first supporting rod 18 is fixed on the inner wall of the vacuum chamber 1, the first supporting rod 18 is horizontally arranged, the other end of the first supporting rod 18 is fixed with one end of the second heat insulation pad 17, and the other end of the second heat insulation pad 17 is fixed with one end of the fixed pressure head 2;
the resistance heating unit 4 is a resistance furnace with a hollow cylinder structure, the resistance heating unit 4 is arranged in the vacuum chamber 1, and the central axis of the resistance heating unit 4 is in the horizontal direction; the resistance heating unit 4 consists of an upper half part 4-1 and a lower half part 4-2, the size and the structure of the upper half part 4-1 and the lower half part 4-2 are completely the same, one side of the upper half part 4-1 and one side of the lower half part 4-2 are hinged together through a hinge 21, and the bottom surface of the lower half part 4-2 is fixed on the inner bottom surface of the vacuum chamber 1 through two supporting legs 20; the centers of two end faces of the resistance heating unit 4 are respectively provided with a through hole, the fixed pressure head 2 is horizontally fixed in one of the through holes, the movable pressure head 5 is arranged in the other through hole, and the movable pressure head 5 and the through holes are in sliding connection; the fixed pressure head 2 and the movable pressure head 5 are arranged oppositely, and one ends of the two pressure heads which are opposite are arranged in the resistance heating unit 4;
the second support rod 19 is horizontally arranged in the vacuum chamber 1, two ends of the second support rod 19 are respectively fixed with one end of the first heat insulation pad 14 and one end of the pressure sensor 12, and the other end of the first heat insulation pad 14 is fixed with one end of the movable pressure head 5; the other end of the pressure sensor 12 is fixed with the power output end of the hydraulic servo transmission device 7, the displacement sensor 6 is arranged on the hydraulic servo transmission device 7, and the power output end of the hydraulic servo transmission device 7 penetrates through the side wall of the vacuum chamber 1 and is in sliding connection and sealing with the side wall of the vacuum chamber 1; the displacement sensor 6 is disposed outside the vacuum chamber 1; the pressure sensor 12 and the first heat insulating pad 14 are both provided inside the vacuum chamber 1; the signal input end of the temperature control device 11 is respectively connected with the signal output ends of the first thermocouple 8, the second thermocouple 9 and the third thermocouple 10; the first thermocouple 8, the second thermocouple 9 and the third thermocouple 10 all penetrate through the vacuum chamber 1 and the resistance heating unit 4; the temperature control device 11 is arranged outside the vacuum chamber 1;
the signal output end of the controller is respectively connected with the signal input end of the hydraulic servo transmission device 7, the signal input end of the resistance heating unit 4 and the signal input end of the vacuumizing device 13; the signal input end of the controller is respectively connected with the signal output ends of the displacement sensor 6 and the pressure sensor 12.
The use method of the device for measuring the semi-solid rheological behavior of the high-entropy alloy comprises the following steps:
the method comprises the following steps: proportioning the high-entropy alloy to be tested according to the designed component element content, smelting the high-entropy alloy into an ingot by using an electromagnetic suspension smelting method, and repeatedly smelting for more than 5 times to finally form a cylindrical ingot with a large section;
step two: processing a cylindrical cast ingot with a large section into a cylindrical sample 3 by utilizing linear cutting;
step three: opening the upper half part 4-1 of the resistance heating device 4, putting a cylindrical sample 3 between the fixed pressure head 2 and the movable pressure head 5, and respectively padding a first graphite gasket 15 and a second graphite gasket 16 at two ends of the cylindrical sample 3; then starting a hydraulic servo transmission device 7 to move a movable pressure head 5 towards the cylindrical sample 3 to compress the cylindrical sample 3 with graphite gaskets at two ends; connecting the testing ends of the first thermocouple 8, the second thermocouple 9 and the third thermocouple 10 with the two ends and the middle of the cylindrical sample 3 respectively;
step four: closing the upper half part 4-1, starting a vacuumizing device 13 to vacuumize the vacuum chamber 1, and then electrifying the resistance heating unit 4 to heat the cylindrical sample 3 to a required temperature;
step five: when the temperatures displayed by the three thermocouples are consistent with the required temperature, starting heat preservation, and when the heat preservation time reaches the required time, starting a hydraulic servo transmission device 7 to move the movable pressure head 5 to the cylindrical sample 3 to finish the compression of the preset deformation epsilon; respectively recording a plurality of pressures F and a plurality of displacement values h corresponding to a plurality of compression time points in the compression process by using a pressure sensor 12 and a displacement sensor 6, and recording a plurality of compression times t by using a timing device;
step six: according to the collected pressure F and the length h of the sample after compressionsThe pressure F and the length h after compression of the sample are plottedsThe relationship curve of (1); h iss＝h0-h，h0The length of the cylinder sample 3 when uncompressed;
step seven: dividing the deformation amount epsilon by the compression time t recorded in the step five to convert the strain rate corresponding to the time t
Calculating the volume V of the cylindrical sample 3 according to a cylindrical volume formula;
d is the end face diameter of the cylindrical sample 3;
step eight: f-h in step sixεFinding the maximum pressure value F in the relation curvemaxAnd its corresponding height h after compression of the cylindrical sample 3maxThen bring both into the formula
And
calculating the apparent viscosity eta corresponding to a plurality of compression time points in the compression processappAnd average shear rate
Step nine: plotting apparent viscosity etaappAnd average shear rate γavAnd (4) a curve is formed, so that the rheological behavior characteristic of the high-entropy alloy in the compression process is obtained.
The invention has the beneficial effects that:
1. the high-entropy alloy rheological behavior measuring device provided by the invention utilizes the structural design of built-in resistance heating of the vacuum chamber 1 and three measuring modes of directly contacting the surface of the sample, can fully monitor and measure the temperature change in the heating process of the high-entropy alloy sample, and fully ensures the uniform heating of the high-entropy alloy measuring sample;
2. the high-entropy alloy rheological behavior measuring device provided by the invention adopts a vacuum chamber design idea, fully considers the technical problem that the high-entropy alloy is easy to oxidize in a semi-solid state, and can fully avoid adverse effects on experiments caused by oxidation by utilizing the vacuum chamber design rheological experimental measurement;
3. the high-entropy alloy rheological behavior measuring device provided by the invention adopts the hydraulic servo transmission mechanism 7 to provide experimental load application, so that the applied displacement precision and load precision can be effectively controlled, and the precision of a high-entropy alloy rheological experiment is ensured;
4. the high-entropy alloy rheological behavior measurement method provided by the invention can effectively measure the rheological behavior of the high solid phase fraction high-entropy alloy semi-solid slurry by utilizing the rheological measurement technical idea of parallel plate compression (the fixed pressure head 2 and the movable pressure head 5), and effectively solves the technical bottleneck problem that the rheological behavior of the high solid phase fraction semi-solid slurry is difficult to measure by the traditional stirring measurement.
Drawings
FIG. 1 is a schematic diagram of a device for measuring semi-solid rheological behavior of a high-entropy alloy according to a first embodiment;
fig. 2 is a sectional view taken along line a-a of fig. 1.
Detailed Description
The first embodiment is as follows: the embodiment is a device for measuring semi-solid rheological behavior of a high-entropy alloy, and as shown in fig. 1 and fig. 2, the device specifically comprises a vacuum chamber 1, a fixed pressure head 2, a resistance heating unit 4, a movable pressure head 5, a displacement sensor 6, a hydraulic servo transmission device 7, a first thermocouple 8, a second thermocouple 9, a third thermocouple 10, a temperature control device 11, a pressure sensor 12, a vacuumizing device 13, a first heat insulation pad 14, a first graphite gasket 15, a second graphite gasket 16, a second heat insulation pad 17, a first support rod 18, a second support rod 19, support legs 20, a hinge 21 and a controller;
the vacuum chamber 1 is communicated with an air exhaust port of a vacuum device 13, and the vacuum device 13 is arranged outside the vacuum chamber 1; one end of the first supporting rod 18 is fixed on the inner wall of the vacuum chamber 1, the first supporting rod 18 is horizontally arranged, the other end of the first supporting rod 18 is fixed with one end of the second heat insulation pad 17, and the other end of the second heat insulation pad 17 is fixed with one end of the fixed pressure head 2;
the resistance heating unit 4 is a resistance furnace with a hollow cylinder structure, the resistance heating unit 4 is arranged in the vacuum chamber 1, and the central axis of the resistance heating unit 4 is in the horizontal direction; the resistance heating unit 4 consists of an upper half part 4-1 and a lower half part 4-2, the size and the structure of the upper half part 4-1 and the lower half part 4-2 are completely the same, one side of the upper half part 4-1 and one side of the lower half part 4-2 are hinged together through a hinge 21, and the bottom surface of the lower half part 4-2 is fixed on the inner bottom surface of the vacuum chamber 1 through two supporting legs 20; the centers of two end faces of the resistance heating unit 4 are respectively provided with a through hole, the fixed pressure head 2 is horizontally fixed in one of the through holes, the movable pressure head 5 is arranged in the other through hole, and the movable pressure head 5 and the through holes are in sliding connection; the fixed pressure head 2 and the movable pressure head 5 are arranged oppositely, and one ends of the two pressure heads which are opposite are arranged in the resistance heating unit 4;
the second support rod 19 is horizontally arranged in the vacuum chamber 1, two ends of the second support rod 19 are respectively fixed with one end of the first heat insulation pad 14 and one end of the pressure sensor 12, and the other end of the first heat insulation pad 14 is fixed with one end of the movable pressure head 5; the other end of the pressure sensor 12 is fixed with the power output end of the hydraulic servo transmission device 7, the displacement sensor 6 is arranged on the hydraulic servo transmission device 7, and the power output end of the hydraulic servo transmission device 7 penetrates through the side wall of the vacuum chamber 1 and is in sliding connection and sealing with the side wall of the vacuum chamber 1; the displacement sensor 6 is disposed outside the vacuum chamber 1; the pressure sensor 12 and the first heat insulating pad 14 are both provided inside the vacuum chamber 1; the signal input end of the temperature control device 11 is respectively connected with the signal output ends of the first thermocouple 8, the second thermocouple 9 and the third thermocouple 10; the first thermocouple 8, the second thermocouple 9 and the third thermocouple 10 all penetrate through the vacuum chamber 1 and the resistance heating unit 4; the temperature control device 11 is arranged outside the vacuum chamber 1;
the signal output end of the controller is respectively connected with the signal input end of the hydraulic servo transmission device 7, the signal input end of the resistance heating unit 4 and the signal input end of the vacuumizing device 13; the signal input end of the controller is respectively connected with the signal output ends of the displacement sensor 6 and the pressure sensor 12.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the vacuum-pumping device 13 is a two-stage vacuum-pumping device of a mechanical pump and a diffusion pump. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the hydraulic servo transmission device 7 adopts a slide valve as a conversion amplification element, the output is displacement, and the control precision of the output displacement is 0.02 mm-0.05 mm. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the speed adjustable range of the hydraulic servo transmission device 7 is 0-500 mm/s. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: the first heat insulation pad 14 is made of asbestos. The rest is the same as the fourth embodiment.
The sixth specific implementation mode: the first difference between the present embodiment and the specific embodiment is: the second heat insulation pad 17 is made of asbestos. The rest is the same as the first embodiment.
The seventh embodiment: the first difference between the present embodiment and the specific embodiment is: the first support rod 18 is made of heat-resistant alloy steel. The rest is the same as the first embodiment.
The specific implementation mode is eight: the first difference between the present embodiment and the specific embodiment is: the second support rod 19 is made of heat-resistant alloy steel. The rest is the same as the first embodiment.
The specific implementation method nine: the first difference between the present embodiment and the specific embodiment is: the length of the resistance heating unit 4 is 120mm, the outer diameter of the end face is 200mm, and the heating power is 2 kw. The rest is the same as the first embodiment.
The detailed implementation mode is ten: the first difference between the present embodiment and the specific embodiment is: the outer diameters of the fixed pressure head 2 and the movable pressure head 5 are both 50 mm. The rest is the same as the first embodiment.
The concrete implementation mode eleven: the first difference between the present embodiment and the specific embodiment is: the first graphite gasket 15 and the second graphite gasket 16 are both phi 10mm and 0.5mm in size. The rest is the same as the first embodiment.
The specific implementation mode twelve: the embodiment is a use method of the high-entropy alloy semi-solid rheological behavior measuring device, which is specifically as follows:
the method comprises the following steps: proportioning the high-entropy alloy to be tested according to the designed component element content, smelting the high-entropy alloy into an ingot by using an electromagnetic suspension smelting method, and repeatedly smelting for more than 5 times to finally form a cylindrical ingot with a large section;
step two: processing a cylindrical cast ingot with a large section into a cylindrical sample 3 by utilizing linear cutting;
step three: opening the upper half part 4-1 of the resistance heating device 4, putting a cylindrical sample 3 between the fixed pressure head 2 and the movable pressure head 5, and respectively padding a first graphite gasket 15 and a second graphite gasket 16 at two ends of the cylindrical sample 3; then starting a hydraulic servo transmission device 7 to move a movable pressure head 5 towards the cylindrical sample 3 to compress the cylindrical sample 3 with graphite gaskets at two ends; connecting the testing ends of the first thermocouple 8, the second thermocouple 9 and the third thermocouple 10 with the two ends and the middle of the cylindrical sample 3 respectively;
step four: closing the upper half part 4-1, starting a vacuumizing device 13 to vacuumize the vacuum chamber 1, and then electrifying the resistance heating unit 4 to heat the cylindrical sample 3 to a required temperature;
step five: when the temperatures displayed by the three thermocouples are consistent with the required temperature, starting heat preservation, and when the heat preservation time reaches the required time, starting a hydraulic servo transmission device 7 to move the movable pressure head 5 to the cylindrical sample 3 to finish the compression of the preset deformation epsilon; respectively recording a plurality of pressures F and a plurality of displacement values h corresponding to a plurality of compression time points in the compression process by using a pressure sensor 12 and a displacement sensor 6, and recording a plurality of compression times t by using a timing device;
step six: according to the collected pressure F and the length h of the sample after compressionsThe pressure F and the length h after compression of the sample are plottedsThe relationship curve of (1); h iss＝h0-h，h0The length of the cylinder sample 3 when uncompressed;
step seven: dividing the deformation amount epsilon by the compression time t recorded in the step five to convert the strain rate corresponding to the time t
Calculating the volume V of the cylindrical sample 3 according to a cylindrical volume formula;
d is the end face diameter of the cylindrical sample 3;
step eight: f-h in step sixεFinding the maximum pressure value F in the relation curvemaxAnd its corresponding height h after compression of the cylindrical sample 3maxThen bring both into the formula
And
calculating the apparent viscosity eta corresponding to a plurality of compression time points in the compression processappAnd average shear rate
Step nine: plotting apparent viscosity etaappAnd average shear rate γavAnd (4) a curve is formed, so that the rheological behavior characteristic of the high-entropy alloy in the compression process is obtained.
The specific implementation mode is thirteen: the present embodiment is twelve different from the specific embodiment: and in the second step, the cylindrical cast ingot with the large section is processed into a cylindrical sample 3 with phi 6mm by 9mm by utilizing linear cutting. The rest is the same as the embodiment twelve.
The specific implementation mode is fourteen: the present embodiment is twelve different from the specific embodiment: in the fourth step, the upper half part 4-1 is closed, the vacuum-pumping device 13 is started to pump the vacuum in the vacuum chamber 1 to the vacuum degree less than 1x10-3Pa. The rest is the same as the embodiment twelve.
The invention was verified with the following tests:
test one: the test is a device for measuring semi-solid rheological behavior of high-entropy alloy, and as shown in fig. 1 and fig. 2, the device specifically comprises a vacuum chamber 1, a fixed pressure head 2, a resistance heating unit 4, a movable pressure head 5, a displacement sensor 6, a hydraulic servo transmission device 7, a first thermocouple 8, a second thermocouple 9, a third thermocouple 10, a temperature control device 11, a pressure sensor 12, a vacuumizing device 13, a first heat insulation pad 14, a first graphite gasket 15, a second graphite gasket 16, a second heat insulation pad 17, a first support rod 18, a second support rod 19, support legs 20, a hinge 21 and a controller; the vacuum-pumping device 13 is a two-stage vacuum-pumping device of a mechanical pump and a diffusion pump; the hydraulic servo transmission device 7 adopts a slide valve as a conversion amplification element, the output is displacement, and the control precision of the output displacement is 0.02 mm-0.05 mm; the speed adjustable range of the hydraulic servo transmission device 7 is 0-500 mm/s; the first heat insulation pad 14 is made of asbestos; the second heat insulation pad 17 is made of asbestos; the first support rod 18 is made of heat-resistant alloy steel; the second support rod 19 is made of heat-resistant alloy steel; the outer diameters of the fixed pressure head 2 and the movable pressure head 5 are both 50 mm; the first graphite gasket 15 and the second graphite gasket 16 are both phi 10mm and 0.5mm in size;
the vacuum chamber 1 is communicated with an air exhaust port of a vacuum device 13, and the vacuum device 13 is arranged outside the vacuum chamber 1; one end of the first supporting rod 18 is fixed on the inner wall of the vacuum chamber 1, the first supporting rod 18 is horizontally arranged, the other end of the first supporting rod 18 is fixed with one end of the second heat insulation pad 17, and the other end of the second heat insulation pad 17 is fixed with one end of the fixed pressure head 2;
the resistance heating unit 4 is a resistance furnace with a hollow cylinder structure, the length of the resistance heating unit 4 is 120mm, the outer diameter of the end face is 200mm, and the heating power is 2 kw; the resistance heating unit 4 is arranged in the vacuum chamber 1, and the central axis of the resistance heating unit 4 is in the horizontal direction; the resistance heating unit 4 consists of an upper half part 4-1 and a lower half part 4-2, the size and the structure of the upper half part 4-1 and the lower half part 4-2 are completely the same, one side of the upper half part 4-1 and one side of the lower half part 4-2 are hinged together through a hinge 21, and the bottom surface of the lower half part 4-2 is fixed on the inner bottom surface of the vacuum chamber 1 through two supporting legs 20; the centers of two end faces of the resistance heating unit 4 are respectively provided with a through hole, the fixed pressure head 2 is horizontally fixed in one of the through holes, the movable pressure head 5 is arranged in the other through hole, and the movable pressure head 5 and the through holes are in sliding connection; the fixed pressure head 2 and the movable pressure head 5 are arranged oppositely, and one ends of the two pressure heads which are opposite are arranged in the resistance heating unit 4;
the second support rod 19 is horizontally arranged in the vacuum chamber 1, two ends of the second support rod 19 are respectively fixed with one end of the first heat insulation pad 14 and one end of the pressure sensor 12, and the other end of the first heat insulation pad 14 is fixed with one end of the movable pressure head 5; the other end of the pressure sensor 12 is fixed with the power output end of the hydraulic servo transmission device 7, the displacement sensor 6 is arranged on the hydraulic servo transmission device 7, and the power output end of the hydraulic servo transmission device 7 penetrates through the side wall of the vacuum chamber 1 and is in sliding connection and sealing with the side wall of the vacuum chamber 1; the displacement sensor 6 is disposed outside the vacuum chamber 1; the pressure sensor 12 and the first heat insulating pad 14 are both provided inside the vacuum chamber 1; the signal input end of the temperature control device 11 is respectively connected with the signal output ends of the first thermocouple 8, the second thermocouple 9 and the third thermocouple 10; the first thermocouple 8, the second thermocouple 9 and the third thermocouple 10 all penetrate through the vacuum chamber 1 and the resistance heating unit 4; the temperature control device 11 is arranged outside the vacuum chamber 1;
the signal output end of the controller is respectively connected with the signal input end of the hydraulic servo transmission device 7, the signal input end of the resistance heating unit 4 and the signal input end of the vacuumizing device 13; the signal input end of the controller is respectively connected with the signal output ends of the displacement sensor 6 and the pressure sensor 12.
The using method of the measuring device for the semi-solid rheological behavior of the high-entropy alloy in the test comprises the following specific steps:
the method comprises the following steps: proportioning the high-entropy alloy to be tested according to the designed component element content, smelting the high-entropy alloy into an ingot by using an electromagnetic suspension smelting method, and repeatedly smelting for more than 5 times to finally form a cylindrical ingot with a large section;
step two: machining a large-size cylindrical cast ingot with a section into a cylindrical sample 3 with phi 6mm x 9mm by utilizing linear cutting;
step three: opening the upper half part 4-1 of the resistance heating device 4, putting a cylindrical sample 3 between the fixed pressure head 2 and the movable pressure head 5, and respectively padding a first graphite gasket 15 and a second graphite gasket 16 at two ends of the cylindrical sample 3; then starting a hydraulic servo transmission device 7 to move a movable pressure head 5 towards the cylindrical sample 3 to compress the cylindrical sample 3 with graphite gaskets at two ends; connecting the testing ends of the first thermocouple 8, the second thermocouple 9 and the third thermocouple 10 with the two ends and the middle of the cylindrical sample 3 respectively;
step four: the upper half part 4-1 is closed, and the vacuum-pumping device 13 is started to pump the vacuum in the vacuum chamber 1 to the vacuum degree less than 1x10-3Pa, then electrifying the resistance heating unit 4 to heat the cylindrical sample 3 to the required temperature;
step five: when the temperatures displayed by the three thermocouples are consistent with the required temperature, starting heat preservation, and when the heat preservation time reaches the required time, starting a hydraulic servo transmission device 7 to move the movable pressure head 5 to the cylindrical sample 3 to finish the compression of the preset deformation epsilon; respectively recording a plurality of pressures F and a plurality of displacement values h corresponding to a plurality of compression time points in the compression process by using a pressure sensor 12 and a displacement sensor 6, and recording a plurality of compression times t by using a timing device;
step six: according to the collected pressure F and the length h of the sample after compressionsThe pressure F and the length h after compression of the sample are plottedsThe relationship curve of (1); h iss＝h0-h，h0The length of the cylinder sample 3 when uncompressed;
step seven: dividing the deformation amount epsilon by the compression time t recorded in the step five to convert the strain rate corresponding to the time t
Calculating the volume V of the cylindrical sample 3 according to a cylindrical volume formula;
d is the end face diameter of the cylindrical sample 3;
step eight: f-h in step sixεFinding the maximum pressure value in the relation curveFmaxAnd its corresponding height h after compression of the cylindrical sample 3maxThen bring both into the formula
And
calculating the apparent viscosity eta corresponding to a plurality of compression time points in the compression processappAnd average shear rate
Step nine: plotting apparent viscosity etaappAnd average shear rate γavAnd (4) a curve is formed, so that the rheological behavior characteristic of the high-entropy alloy in the compression process is obtained.
The beneficial effect of this experiment is:
1. the high-entropy alloy rheological behavior measuring device provided by the test utilizes the structural design of built-in resistance heating of the vacuum chamber 1 and three measuring modes of directly contacting the surface of the sample, can fully monitor and measure the temperature change in the heating process of the high-entropy alloy sample, and fully ensures the uniform heating of the high-entropy alloy measuring sample;
2. the high-entropy alloy rheological behavior measuring device provided by the test adopts a vacuum chamber design idea, fully considers the technical problem that the high-entropy alloy is easy to oxidize in a semi-solid state, and can fully avoid adverse effects on the test caused by oxidation by utilizing the vacuum chamber design rheological experimental measurement;
3. the high-entropy alloy rheological behavior measuring device provided by the test adopts the hydraulic servo transmission mechanism 7 to provide test load application, so that the applied displacement precision and load precision can be effectively controlled, and the precision of the high-entropy alloy rheological test is ensured;
4. the high-entropy alloy rheological behavior measurement method provided by the test utilizes the rheological measurement technical idea of parallel plate compression (the fixed pressure head 2 and the movable pressure head 5), can effectively measure the rheological behavior of the high-solid-phase-fraction high-entropy alloy semi-solid slurry, and effectively solves the technical bottleneck problem that the traditional stirring measurement is difficult to measure the rheological behavior of the high-solid-phase-fraction semi-solid slurry.
Claims (14)
1. The device for measuring the semi-solid rheological behavior of the high-entropy alloy is characterized by consisting of a vacuum chamber (1), a fixed pressure head (2), a resistance heating unit (4), a movable pressure head (5), a displacement sensor (6), a hydraulic servo transmission device (7), a first thermocouple (8), a second thermocouple (9), a third thermocouple (10), a temperature control device (11), a pressure sensor (12), a vacuumizing device (13), a first heat insulation pad (14), a first graphite gasket (15), a second graphite gasket (16), a second heat insulation pad (17), a first supporting rod (18), a second supporting rod (19), supporting legs (20), hinges (21) and a controller;
the vacuum chamber (1) is communicated with an air extraction opening of a vacuum extractor (13), and the vacuum extractor (13) is arranged outside the vacuum chamber (1); one end of the first supporting rod (18) is fixed on the inner wall of the vacuum chamber (1), the first supporting rod (18) is horizontally arranged, the other end of the first supporting rod (18) is fixed with one end of the second heat insulation pad (17), and the other end of the second heat insulation pad (17) is fixed with one end of the fixed pressure head (2);
the resistance heating unit (4) is a resistance furnace with a hollow cylinder structure, the resistance heating unit (4) is arranged in the vacuum chamber (1), and the central axis of the resistance heating unit (4) is in the horizontal direction; the resistance heating unit (4) consists of an upper half part (4-1) and a lower half part (4-2), the size and the structure of the upper half part (4-1) and the lower half part (4-2) are completely the same, one side of the upper half part (4-1) and one side of the lower half part (4-2) are hinged together through a hinge (21), and the bottom surface of the lower half part (4-2) is fixed on the inner bottom surface of the vacuum chamber 1 through two supporting legs (20); the centers of two end faces of the resistance heating unit (4) are respectively provided with a through hole, the fixed pressure head (2) is horizontally fixed in one of the through holes, the movable pressure head (5) is arranged in the other through hole, and the movable pressure head (5) is in sliding connection with the through holes; the fixed pressure head (2) and the movable pressure head (5) are arranged oppositely, and one ends of the two pressure heads which are opposite are arranged in the resistance heating unit (4);
the second supporting rod (19) is horizontally arranged in the vacuum chamber (1), two ends of the second supporting rod (19) are respectively fixed with one end of the first heat insulation pad (14) and one end of the pressure sensor (12), and the other end of the first heat insulation pad (14) is fixed with one end of the movable pressure head (5); the other end of the pressure sensor (12) is fixed with the power output end of the hydraulic servo transmission device (7), the displacement sensor (6) is arranged on the hydraulic servo transmission device (7), and the power output end of the hydraulic servo transmission device (7) penetrates through the side wall of the vacuum chamber (1) and is in sliding connection and sealing with the side wall of the vacuum chamber (1); the displacement sensor (6) is arranged outside the vacuum chamber (1); the pressure sensor (12) and the first heat insulation pad (14) are arranged inside the vacuum chamber (1); the signal input end of the temperature control device (11) is respectively connected with the signal output ends of the first thermocouple (8), the second thermocouple (9) and the third thermocouple (10); the first thermocouple (8), the second thermocouple (9) and the third thermocouple (10) penetrate through the vacuum chamber (1) and the resistance heating unit (4); the temperature control device (11) is arranged outside the vacuum chamber (1);
the signal output end of the controller is respectively connected with the signal input end of the hydraulic servo transmission device (7), the signal input end of the resistance heating unit (4) and the signal input end of the vacuumizing device (13); the signal input end of the controller is respectively connected with the signal output ends of the displacement sensor (6) and the pressure sensor (12).
2. A device for measuring semi-solid rheological behavior of a high-entropy alloy according to claim 1, wherein the evacuating device (13) is a two-stage evacuating device of a mechanical pump and a diffusion pump.
3. A high-entropy alloy semi-solid rheological behavior measuring device according to claim 1, characterized in that the hydraulic servo transmission device (7) adopts a slide valve as a conversion amplification element, the output is displacement, and the control precision of the output displacement is 0.02 mm-0.05 mm.
4. A device for measuring semi-solid rheological behavior of a high-entropy alloy according to claim 1, wherein the speed of the hydraulic servo transmission device (7) is adjustable within a range of 0-500 mm/s.
5. A device for measuring semi-solid rheological behavior of a high-entropy alloy according to claim 1, wherein the first insulating mat (14) is made of asbestos.
6. A device for measuring semi-solid rheological behavior of a high-entropy alloy according to claim 1, wherein the second heat insulating mat (17) is made of asbestos.
7. A device for measuring semi-solid rheological behavior of a high-entropy alloy according to claim 1, wherein the first support rod (18) is made of heat-resistant alloy steel.
8. A device for measuring semi-solid rheological behavior of a high-entropy alloy according to claim 1, wherein the second support rod (19) is made of heat-resistant alloy steel.
9. A high entropy alloy semi-solid state rheological behavior measuring device according to claim 1, characterized in that the length of the resistance heating unit (4) is 120mm, the end face outer diameter is 200mm, and the heating power is 2 kw.
10. A device for measuring semi-solid rheological behavior of a high-entropy alloy according to claim 1, wherein the fixed ram (2) and the movable ram (5) both have an outer diameter of 50 mm.
11. A device for measuring semi-solid rheological behavior of a high-entropy alloy, according to claim 1, wherein the first graphite gasket (15) and the second graphite gasket (16) each have a dimension Φ 10mm x 0.5 mm.
12. The use method of the device for measuring the semi-solid rheological behavior of the high-entropy alloy as claimed in claim 1, is characterized in that the use method of the device for measuring the semi-solid rheological behavior of the high-entropy alloy is as follows:
the method comprises the following steps: proportioning the high-entropy alloy to be tested according to the designed component element content, smelting the high-entropy alloy into an ingot by using an electromagnetic suspension smelting method, and repeatedly smelting for more than 5 times to finally form a cylindrical ingot with a large section;
step two: processing a large-size cylindrical cast ingot with a section into a cylindrical sample (3) by utilizing linear cutting;
step three: opening the upper half part (4-1) of the resistance heating device (4), putting a cylindrical sample (3) between the fixed pressure head (2) and the movable pressure head (5), and respectively padding a first graphite gasket (15) and a second graphite gasket (16) at two ends of the cylindrical sample (3); then starting a hydraulic servo transmission device (7) to move a movable pressure head (5) towards the cylindrical sample (3) to compress the cylindrical sample (3) with graphite gaskets at two ends; respectively connecting the testing ends of the first thermocouple (8), the second thermocouple (9) and the third thermocouple (10) with the two ends and the middle of the cylindrical sample (3);
step four: closing the upper half part (4-1), starting a vacuumizing device (13) to vacuumize the vacuum chamber (1), and then electrifying the resistance heating unit (4) to heat the cylindrical sample (3) to a required temperature;
step five: when the temperatures displayed by the three thermocouples are consistent with the required temperature, starting heat preservation, and when the heat preservation time reaches the required time, starting a hydraulic servo transmission device (7) to move a movable pressure head (5) to the cylindrical sample (3) to finish the compression of the preset deformation epsilon; respectively recording a plurality of pressures F and a plurality of displacement values h corresponding to a plurality of compression time points in the compression process by using a pressure sensor (12) and a displacement sensor (6), and recording a plurality of compression times t by using a timing device;
step six: according to the collected pressure F and the length h of the sample after compressionsThe pressure F and the length h after compression of the sample are plottedsThe relationship curve of (1); h iss＝h0-h，h0The length of the cylinder sample (3) when not compressed;
step seven: dividing the deformation amount epsilon by the compression time t recorded in the step five to convert the strain corresponding to the time tRate of speed
Calculating the volume V of the cylindrical sample (3) according to a cylindrical volume formula;
d is the diameter of the end face of the cylindrical sample (3);
step eight: f-h in step sixεFinding the maximum pressure value F in the relation curvemaxAnd its corresponding height h after compression of the cylindrical sample 3maxThen bring both into the formula
And
calculating the apparent viscosity eta corresponding to a plurality of compression time points in the compression processappAnd average shear rate
Step nine: plotting apparent viscosity etaappAnd average shear rate γavAnd (4) a curve is formed, so that the rheological behavior characteristic of the high-entropy alloy in the compression process is obtained.
13. A method for using the device for measuring semi-solid rheological behavior of the high-entropy alloy according to claim 12, wherein the second step is to process the cylindrical ingot with large section size into the cylindrical sample (3) with phi 6mm x 9mm by using wire cutting.
14. Use method of the device for measuring semi-solid rheological behavior of high-entropy alloy according to claim 12, characterized in that the step fourThe upper half part (4-1) is closed, and the vacuum-pumping device (13) is started to pump the vacuum in the vacuum chamber (1) to the vacuum degree of less than 1x10-3Pa。
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