CN112326714A - Device and method for measuring Curie temperature of magnetic material - Google Patents
Device and method for measuring Curie temperature of magnetic material Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000000696 magnetic material Substances 0.000 title claims abstract description 24
- 239000000919 ceramic Substances 0.000 claims abstract description 85
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- 238000010438 heat treatment Methods 0.000 claims abstract description 44
- 238000005259 measurement Methods 0.000 claims abstract description 39
- 230000007246 mechanism Effects 0.000 claims abstract description 20
- 238000004804 winding Methods 0.000 claims abstract description 19
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 12
- 230000006698 induction Effects 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 10
- 238000012360 testing method Methods 0.000 description 12
- 230000001276 controlling effect Effects 0.000 description 11
- 229910045601 alloy Inorganic materials 0.000 description 10
- 239000000956 alloy Substances 0.000 description 10
- 238000001514 detection method Methods 0.000 description 10
- 230000008859 change Effects 0.000 description 6
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
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- 238000009529 body temperature measurement Methods 0.000 description 2
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- 230000005674 electromagnetic induction Effects 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000005408 paramagnetism Effects 0.000 description 1
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Abstract
The invention discloses a measuring device for Curie temperature of a magnetic material, which comprises: heating furnace; a temperature controller; the surface is provided with a ceramic sample box with P circles of grooves; the excitation lead is used for winding M turns of excitation coils in the groove of the ceramic sample box; the measuring lead is used for winding N turns of measuring coils in the groove of the ceramic sample box; the thermocouple is used for measuring the temperature of a sample to be measured, and a lead of the thermocouple is connected with a temperature controller; the hollow connecting rod is arranged in the hearth and used for leading the excitation lead and the measurement lead out of the hearth; the voltage measuring mechanism is connected with the measuring lead and is used for measuring the induced voltage of the sample to be measured; the excitation signal source is connected with the excitation lead wire and used for providing excitation current in the measuring process; the measuring device ensures that the coils of adjacent turns cannot generate short circuit due to overlapping, and ensures the accuracy of the measuring and detecting result.
Description
Technical Field
The application relates to the technical field of magnetic material performance detection, in particular to a measuring device and a measuring method for Curie temperature of a magnetic material.
Background
The Curie temperature is the critical transition temperature of the material from ferromagnetism to paramagnetism, is an important parameter for measuring the temperature stability of the magnetic material, and directly influences the application of the material in industrial engineering. Taking soft magnetic materials as an example, the soft magnetic materials are widely used due to the characteristics of high magnetic permeability, low coercive force, low loss and the like, and are one of the materials with large usage amount in magnetic materials. The Curie temperature is one of important characteristic parameters of the soft magnetic material, and accurate and efficient measurement has important significance for guiding research and application of the material. The curie temperature measurement method is divided into a plurality of measurement principles and measurement modes, common measurement methods include an induction method, a resonance method, an electric bridge method, a magnetic scale method, a DSC and the like, and the induction method is widely applied due to accurate, convenient and fast measurement.
When the Curie temperature is measured by an induction method, an excitation coil and a measuring coil with preset turns are required to be wound on a sample to be measured of a magnetic material, the measuring coil is also called an induction coil, when the Curie temperature is measured, exciting current is continuously introduced into the excitation coil in the temperature rising process, then induced electromotive force of the measuring coil is detected, a curve of induced electromotive force changing along with the temperature is obtained, then the maximum slope of the curve is obtained by a tangent method, and the temperature value corresponding to the maximum slope point is the Curie temperature value of the magnetic material. Because the curie temperature is measured under the high temperature condition, the wire for winding the magnet exciting coil or the induction coil is very easy to be oxidized, the surface insulating layer is dropped off, the coils are overlapped, the number of turns of the coils is changed, the accuracy of induction voltage data is influenced, and further the curie temperature measurement result is influenced.
Disclosure of Invention
The invention provides a measuring device and a measuring method for Curie temperature of a magnetic material, and aims to solve or partially solve the technical problems that after a measuring coil is oxidized at high temperature and a surface insulating layer falls off, the coil is easy to overlap, and the accuracy of test data is influenced.
In order to solve the above technical problem, the present invention provides a device for measuring curie temperature of a magnetic material, comprising:
the heating furnace comprises a hearth;
the temperature controller is used for controlling the temperature of the heating furnace;
the surface is provided with a ceramic sample box with P circles of grooves; wherein, the ceramic sample box is placed in a temperature equalizing zone of a hearth after a sample to be detected is placed in the ceramic sample box, and P is more than or equal to 4;
the excitation lead is used for winding M turns of excitation coils in the groove of the ceramic sample box, wherein M is more than or equal to 2;
the measuring lead is used for winding N measuring coils in the groove of the ceramic sample box, wherein N is more than or equal to 2;
the thermocouple is used for measuring the temperature of a sample to be measured; the lead of the thermocouple is connected with a temperature controller;
the hollow connecting rod is arranged in the hearth and used for leading the excitation lead and the measurement lead out of the hearth;
the voltage measuring mechanism is connected with the measuring lead and is used for measuring the induced voltage of the sample to be measured;
and the excitation signal source is connected with the excitation lead wire and used for providing excitation current in the measurement process.
Optionally, the measuring device further comprises a data collecting mechanism, and the data collecting mechanism is connected with the temperature controller and the voltage measuring mechanism and used for collecting temperature data and induced voltage data.
Optionally, the value range of P is 24-30.
Optionally, the ceramic sample box is provided with a lead hole.
Optionally, the connecting rod is a ceramic connecting rod.
Optionally, the ceramic sample cartridge is an annular sample cartridge.
Furthermore, the inner diameter of the ceramic sample box is 12-16 mm, and the outer diameter of the ceramic sample box is 26-34 mm.
Based on the inventive concept of the foregoing technical solution, the present invention further provides a method for measuring curie temperature of a magnetic material, wherein the measuring device in the foregoing technical solution is adopted, and the measuring method includes:
placing a sample to be detected into a ceramic sample box, wherein the ceramic sample box is positioned in a uniform temperature zone of a hearth, M turns of excitation coils and N turns of measuring coils are wound on the ceramic sample box, and a thermocouple is arranged on the ceramic sample box;
determining a heating process and excitation parameters, controlling the heating furnace to heat up by the temperature controller according to the heating process, and outputting excitation current by the excitation signal source according to the excitation parameters;
acquiring temperature data and induction voltage data of a sample to be detected in a heating process;
and determining the Curie temperature of the sample to be detected according to the temperature data and the induced voltage data.
Optionally, determining the curie temperature of the sample to be measured according to the temperature data and the induced voltage data, specifically including:
fitting by taking the temperature data as an X axis and the induced voltage data as a Y axis to obtain an induced voltage-temperature fitting curve;
solving a first derivative of the induction voltage-temperature fitting curve;
and determining the temperature value corresponding to the maximum value in the first-order derivative as the Curie temperature of the sample to be measured.
Optionally, if the sample to be detected is an annular forged material sample or a plate sample, controlling the inner diameter of the sample to be detected to be more than or equal to 18mm, the outer diameter of the sample to be detected to be less than or equal to 24mm, and controlling the total height of the sample to be detected to be less than or equal to 10 mm;
and if the sample to be detected is a sheet sample, controlling the width of the sample to be detected to be less than 10mm and the thickness of the sample to be detected to be 5-10 mm.
Through one or more technical schemes of the invention, the invention has the following beneficial effects or advantages:
the invention provides a measuring device for Curie temperature of a magnetic material, which comprises: the heating furnace and the temperature controller are used for heating the sample to be measured; placing a sample to be detected in a ceramic sample box with a P-ring groove on the surface; winding an excitation lead into M turns of excitation coils in a groove of the ceramic sample box; winding a measuring lead wire into N turns of measuring coils in the groove of the ceramic sample box; leading the lead wire of the thermocouple, the excitation lead wire and the measurement lead wire out of the hearth by using a connecting rod; wherein, the lead of the thermocouple is connected with a temperature controller; the measuring lead is connected with the voltage measuring mechanism and the excitation lead is connected with the excitation signal source; according to the measuring device, the coil is wound in the groove of the ceramic sample box, even if the insulating layer on the outer layer of the coil is oxidized and falls off after multiple times of measurement, the phenomenon that the coil of adjacent turns is overlapped to generate short circuit can be avoided, so that the stability in the detection process is improved, and the accuracy of the detection result is ensured.
The foregoing description is only an overview of the technical solutions of the present invention, and the embodiments of the present invention are described below in order to make the technical means of the present invention more clearly understood and to make the above and other objects, features, and advantages of the present invention more clearly understandable.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 shows a schematic view of a measurement device according to one embodiment of the invention;
FIG. 2 shows a front view of a ceramic sample cartridge according to one embodiment of the invention;
FIG. 3 shows a top view of a ceramic sample cartridge according to one embodiment of the invention;
FIG. 4 shows a schematic structural view of a connecting rod according to one embodiment of the present invention;
FIG. 5 shows a first derivative curve of U-T for magnetically soft alloy 1 according to an embodiment of the present invention;
FIG. 6 shows a first derivative curve of U-T for magnetically soft alloy 2 according to an embodiment of the present invention;
description of reference numerals:
1. heating furnace; 11. a hearth; 2. a ceramic sample cartridge; 21. a wire hole; 3. a field coil; 4. a measuring coil; 5. thermocouple, 6, connecting rod; 7. a temperature controller; 8. a voltage measuring mechanism; 9. an excitation signal source; 10. a data acquisition mechanism.
Detailed Description
In order to make the present application more clearly understood by those skilled in the art to which the present application pertains, the following detailed description of the present application is made with reference to the accompanying drawings by way of specific embodiments. Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control. Unless otherwise specifically stated, various apparatuses and the like used in the present invention are either commercially available or can be prepared by existing methods.
In order to solve the problems that the measuring coil or the induction coil is oxidized in a high-temperature environment, the surface insulating layer falls off, coil overlapping easily occurs, and the accuracy of the measuring result is affected, in an alternative embodiment, as shown in fig. 1, there is provided a measuring device for the curie temperature of a magnetic material, comprising:
the heating furnace 1, the heating furnace 1 includes the burner hearth 11;
a temperature controller 7 for controlling the temperature of the heating furnace 1;
the surface is provided with a ceramic sample box 2 with P circles of grooves; wherein, the ceramic sample box 2 is placed in a temperature equalizing zone of the hearth 11 after a sample to be detected is placed, and P is more than or equal to 4;
the excitation lead is used for winding an excitation coil 3 with M turns in the groove of the ceramic sample box 2, wherein M is more than or equal to 2;
the measuring lead is used for winding N turns of measuring coils 4 in the groove of the ceramic sample box 2, wherein N is more than or equal to 2;
the thermocouple 5 is used for measuring the temperature of a sample to be measured, and a lead of the thermocouple 5 is connected with a temperature controller 7;
the hollow connecting rod 6 is arranged in the hearth 11 and is used for leading the excitation lead and the measurement lead out of the hearth 11;
the voltage measuring mechanism 8 is connected with the measuring lead wire and is used for measuring the induced voltage of the sample to be measured;
and the excitation signal source 9 is connected with an excitation lead wire and used for providing excitation current in the measurement process.
Specifically, the heating furnace 1 is used for heating a sample to be measured, and the ceramic sample box 2 is filled with the sample to be measured and is arranged in a uniform temperature zone of a hearth 11 of the heating furnace 1. The heating furnace 1 is controlled by a temperature controller 7 (temperature controller for short) to rise to the target temperature according to a preset temperature rise rate. In the measuring process, the excitation signal source 9 outputs excitation (excitation) current, an excitation magnetic field is generated through the excitation coil 3, and the measurement coil 4 is externally connected with the voltage measuring mechanism 8, so that the induced electromotive force of the sample to be measured can be obtained.
Optionally, the excitation lead and the measurement lead may use enameled wires, and the measurement apparatus in this embodiment uses two enameled wires, one of which is used for winding the excitation coil 3 and the other is used for winding the measurement coil 4. Two sets of coils should even coiling on ceramic sample box 2, through with in the enameled wire coiling recess on ceramic sample box 2, can ensure even the insulating layer of enameled wire after the oxidation drops, excitation coil 3 or measurement coil 4 can not overlap joint each other and produce short circuit, the number of turns change yet. Optionally, the value range of P is 24-30, namely the number of the bus coils which can be wound on the ceramic sample box 2 is 24-30, and the excitation coil 3 and the measurement coil 4 can be respectively wound on the groove for 12-15 coils.
Optionally, the groove is a toothed groove.
Optionally, the ceramic sample box 2 is provided with a lead hole 21; the enameled wire passes through the lead hole 21 and then is wound in a groove wound on the ceramic sample box 2. The lead holes 21 are 2 pairs and 4 in total and distributed in the diameter direction of the ceramic sample box 2; the excitation lead and the measurement lead are respectively passed through a pair of lead holes 21 to perform coil winding.
Alternatively, the ceramic sample case 2 may be ring-shaped, square-shaped or other shapes, which are determined according to the shape of the sample to be measured. Optionally, fig. 2 to 3 show an annular ceramic sample box 2, which can be used for measuring an annular sample to be measured, and the ceramic sample box 2 can adopt a vertically split structure, so that the annular sample to be measured is sleeved in the middle of the ceramic sample box 2. The inner diameter of the ceramic sample box is 12-16 mm, and the outer diameter of the ceramic sample box is 26-34 mm; the height is 12 mm-18 mm. The sizes of the samples to be measured applicable to the annular ceramic sample box 2 are as follows: if the sample to be detected is an annular forged material sample or a plate sample, controlling the inner diameter of the sample to be detected to be more than or equal to 18mm, the outer diameter to be less than or equal to 24mm and the total height of the sample to be detected to be less than or equal to 10 mm; and if the sample to be detected is a sheet sample, controlling the width of the sample to be detected to be less than 10mm and the thickness of the sample to be detected to be 5-10 mm.
Optionally, the ceramic sample box 2 can be made of alumina and can be used within the range of 0-1000 ℃; if a higher use temperature is required, a corundum (alumina) ceramic of 99% purity can be selected.
As shown in fig. 4, the connecting rod 6 is optionally a high temperature resistant ceramic connecting rod. The connecting rod 6 is used for protecting and regulating an excitation lead and a measurement lead in a hearth 11 of the heating furnace 1 and leading the leads out of the heating furnace 1; because the excitation lead and the measurement lead can be divided into two lead sections of lead-in lead and lead-out lead after being wound into a coil, the lead sections are four, and simultaneously, in order to prevent the lead from being lapped and short-circuited, at least 4 axial through holes can be arranged in the connecting rod 6, and one lead section passes through one axial through hole. Similarly, the ceramic connecting rod may be made of alumina.
Alternatively, the thermocouple 5 may use a k-type thermocouple or an s-type thermocouple, and a measurement head of the thermocouple 5 may be placed in the middle of the ceramic sample box 2, or a sample may be fixed on the surface of the sample, so as to accurately measure the furnace temperature at the sample to be measured.
Alternatively, the voltage measuring means 8 may be a digital multimeter.
At present, in the Curie temperature measuring process, a detection person needs to record the temperature and the change of the induction voltage point by point, so that a large amount of manpower is consumed, the operation is complex, and the working efficiency is low. Based on this, optionally, the measuring device further includes a data acquisition mechanism 10, and the data acquisition mechanism 10 is connected to the temperature controller 7 and the voltage measurement mechanism 8, and is used for acquiring temperature data and induced voltage data.
Specifically, the data acquisition mechanism 10 is a data acquisition peripheral equipped with matched data acquisition software, induced electromotive force generated by the measuring coil 4 is subjected to signal processing and then fed back to the data acquisition mechanism 10 together with a temperature signal of the thermocouple 5, so that automatic acquisition and recording of temperature and induced voltage data are realized, the labor cost is reduced, and the detection efficiency is improved.
In summary, the present embodiment provides a device for measuring curie temperature of a magnetic material, including: the heating furnace and the temperature controller are used for heating the sample to be measured; placing a sample to be detected in a ceramic sample box with a P-ring groove on the surface; winding an excitation lead into M turns of excitation coils in a groove of the ceramic sample box; winding a measuring lead wire into N turns of measuring coils in the groove of the ceramic sample box; leading the lead wire of the thermocouple, the excitation lead wire and the measurement lead wire out of the hearth by using a connecting rod; wherein, the lead of the thermocouple is connected with a temperature controller; the measuring lead is connected with the voltage measuring mechanism and the excitation lead is connected with the excitation signal source; according to the measuring device, the coil is wound in the groove of the ceramic sample box, even if the insulating layer on the outer layer of the coil is oxidized and falls off after multiple times of measurement, the phenomenon that the coil of adjacent turns is overlapped to generate short circuit can be avoided, so that the stability in the detection process is improved, and the accuracy of the detection result is ensured.
Based on the same inventive concept of the foregoing embodiment, in yet another alternative embodiment, there is provided a method for measuring the curie temperature of a magnetic material, using the measuring apparatus in the foregoing embodiment, the method comprising:
s1: placing a sample to be detected into a ceramic sample box, wherein the ceramic sample box is positioned in a uniform temperature zone of a hearth, M turns of excitation coils and N turns of measuring coils are wound on the ceramic sample box, and a thermocouple is arranged on the ceramic sample box;
s2: determining a heating process and excitation parameters, controlling the heating furnace to heat up by the temperature controller according to the heating process, and outputting excitation current by the excitation signal source according to the excitation parameters;
s3: acquiring temperature data and induction voltage data of a sample to be detected in a heating process;
s4: and determining the Curie temperature of the sample to be detected according to the temperature data and the induced voltage data.
It should be noted that the curie temperature is obtained by a tangent method by measuring the variation curve of the magnetization M with the temperature T during the measurement process by the induction method. In practical detection, an M-T curve can not be accurately obtained generally, and according to the knowledge of the theory of electromagnetism, the change curve of the M-T is similar to that of the B-T, and according to the electromagnetic induction principle
Measuring the induced electromotive force with temperatureAnd (3) drawing a tangent at the position with the maximum slope of the curve with the degree change, wherein the intersection point of the tangent and the abscissa (T) is the Curie temperature of the sample. When the tangent method is used for analyzing the test result, the requirement on the analysis and judgment capability of a tester is high, the maximum slope of the curve needs to be accurately judged, and the operation on a complex curve is relatively difficult.
Therefore, optionally, step S4: according to the temperature data and the induced voltage data, determining the Curie temperature of the sample to be detected, and specifically comprising the following steps:
fitting by taking the temperature data as an X axis and the induced voltage data as a Y axis to obtain an induced voltage-temperature fitting curve;
solving a first derivative of the induction voltage-temperature fitting curve;
and determining the temperature value corresponding to the maximum value in the first-order derivative as the Curie temperature of the sample to be measured.
Specifically, taking a soft magnetic material as an example, the complete measurement process is as follows:
the method comprises the following steps: sample preparation. And (3) putting the sample into a ceramic sample box, wherein the upper and lower lead holes of the ceramic sample box are arranged at two ends of a certain diameter of the protective box. Two enamelled wires with a length of at least 1.5m are prepared, one as an excitation coil and one as a measuring coil. Two threads penetrate through the lead hole to be wound, and two groups of windings are uniformly wound on the protective box without lap joints. And can be wound by 9-12 turns respectively.
Step two: 4 leading wires of the excitation coil and the measuring coil penetrate through the high-temperature ceramic connecting rod, meanwhile, the measuring end of the K-type thermocouple is arranged at the center of the sample, the leading wire of the thermocouple is fixed on the high-temperature ceramic connecting rod, the ceramic sample box filled with the sample to be measured is arranged in the uniform temperature area of the hearth of the heating furnace, and the opening of the high-temperature heating furnace is sealed.
Step three: and connecting the excitation lead with the output end of the signal source, and connecting the measurement lead with the digital multimeter.
Step four: and opening the temperature controller, and setting the test temperature and the test speed. The test highest temperature is at least 50 ℃ higher than the estimated Curie temperature of the soft magnetic material, and the temperature rise rate is preferably controlled to be 5-15 ℃/min.
Step five: and opening data acquisition software, setting sample information, clicking to start, and simultaneously pressing a start button of the temperature controller.
Step six: when the induced voltage in the data acquisition curve is obviously reduced along with the temperature rise and has no obvious change along with the temperature rise, the heating temperature is shown to reach the Curie temperature point of the sample, the data is stored, the heating furnace is closed, and the heating is stopped.
Step seven: and opening data processing software, importing the measured data to be analyzed to perform data fitting of a U-T curve, then performing first derivation on the U-T curve to draw a U' -T first derivation curve, determining the maximum value of dU/dT from the first derivation curve, and determining the corresponding temperature point as the Curie temperature of the sample to be measured.
The U-T functional relation and the curve are fitted through data acquisition software, and then the data are analyzed and processed in a first-order derivation mode to obtain a result.
During measurement, if the sample to be measured is an annular forged material sample or a plate sample, controlling the inner diameter of the sample to be measured to be more than or equal to 18mm, the outer diameter to be less than or equal to 24mm and the total height of the sample to be measured to be less than or equal to 10 mm;
and if the sample to be detected is a sheet sample, controlling the width of the sample to be detected to be less than 10mm and the thickness of the sample to be detected to be 5-10 mm.
In the following embodiments, the technical solutions in the above embodiments are completely described with reference to specific test cases:
in an alternative embodiment, the curie temperature of the soft magnetic alloy 1 wrought material is measured as follows:
1. alloy 1 in a forging material state is processed into an annular sample with the inner diameter of 18mm, the outer diameter of 24mm and the height of 10mm, the sample is placed into a ceramic protective box, and two groups of coils are wound by two enameled wires with the length of 1.5m along the tooth opening of the ceramic protective box.
2. 4 leading wires of 2 groups of coils penetrate through the high-temperature ceramic connecting rod, meanwhile, the measuring end of the K-type thermocouple is arranged at the center of the sample, the thermocouple leading wire is fixed on the high-temperature ceramic connecting rod, the sample bound with the thermocouple is arranged in the temperature equalizing area of the high-temperature heating furnace, and the furnace mouth of the high-temperature heating furnace is sealed.
3. A temperature controller is opened to set a temperature rising program, the Curie temperature estimated value of the alloy is 360 ℃, so the program sets the maximum temperature to be 450 ℃ and the temperature rising rate to be 8 ℃/min.
4. And opening data acquisition software, setting sample information, clicking to start, and simultaneously pressing a start button of the temperature controller.
5. And (4) observing a data acquisition curve, obviously reducing the curve when the temperature is about 340 ℃, storing test data when the induction voltage does not obviously change along with the temperature rise, closing the heating furnace, and stopping the test.
6. The measured data (part of the test data is shown in table 1) is imported into Origin data processing software, wherein the induced voltage is a sequence A, the temperature is a sequence B, the sequence AB is selected to click PLOT-LINE, so that the data fitting of a U-T curve is completed, the analysis-physics-diff experimental-open dialog is clicked, 1 is selected from derivative, so that a first derivative is obtained, a data sequence C is formed after the click OK, the data sequence A, C is selected, the PLOT-LINE is clicked, so that a U-T first derivative curve is formed, the temperature point corresponding to the maximum value of dU/dT in the curve is the Curie temperature of the sample, and the Curie temperature of the analyzed alloy 1 is 348 ℃, as shown in fig. 4.
In a further alternative embodiment, the curie temperature of the soft magnetic alloy 2 strip is measured as follows:
1. the strip alloy 2 having a thickness of 0.15mm was processed into a strip having a width of 10mm, and the upper and lower portions of the ceramic sheath were fixed with an adhesive tape, as shown in FIG. 2. The sample was wound along the inside of the protective case to a thickness of 5mm, and the tape was fixed at the joint. Two groups of coils are wound by using two enameled wires with the length of 1.5m along the tooth opening of the ceramic protection box.
2. 4 leading wires of 2 groups of coils penetrate through the high-temperature ceramic connecting rod, meanwhile, the measuring end of the K-type thermocouple is arranged at the center of the sample, the thermocouple leading wire is fixed on the high-temperature ceramic connecting rod, the sample bound with the thermocouple is arranged in a temperature equalizing area of a high-temperature heating furnace, and a furnace mouth of the high-temperature heating furnace is sealed.
3. A temperature controller is opened to set a temperature rising program, the Curie temperature estimated value of the alloy is 760 ℃, so the program sets the maximum temperature to be 850 ℃ and the temperature rising rate to be 10 ℃/min.
4. And opening data acquisition software, setting sample information, clicking to start, and simultaneously pressing a start button of the temperature controller.
5. And observing a data acquisition curve, when the temperature is about 760 ℃, the curve is obviously reduced, and when the induced voltage is not obviously changed along with the temperature rise, the test data are stored, the heating furnace is closed, and the test is stopped.
6. The measured data (part of the test data is shown in table 1) is introduced into Origin data processing software, wherein the induced voltage is a sequence A, the temperature is a sequence B, the sequence AB is selected to click PLOT-LINE, so that the data fitting of a U-T curve is completed, the analysis-physics-differential-ate-open dialog is clicked, 1 is selected from derivative, so that a first derivative is obtained, a data sequence C is formed after clicking OK, the data sequence A, C is selected, the PLOT-LINE is clicked, so that a U-T first derivative curve is formed, the temperature point corresponding to the maximum value of dU/dT in the curve is the Curie temperature of the sample, and the Curie temperature of the analyzed alloy 1 is 764 ℃, as shown in fig. 5.
TABLE 1 partial measurement raw data for alloy 1 and alloy 2
Through one or more embodiments of the present invention, the present invention has the following advantageous effects or advantages:
the invention provides a measuring device for Curie temperature of a magnetic material, which comprises: the heating furnace and the temperature controller are used for heating the sample to be measured; placing a sample to be detected in a ceramic sample box with a P-ring groove on the surface; winding an excitation lead into M turns of excitation coils in a groove of the ceramic sample box; winding a measuring lead wire into N turns of measuring coils in the groove of the ceramic sample box; leading the lead wire of the thermocouple, the excitation lead wire and the measurement lead wire out of the hearth by using a connecting rod; wherein, the lead of the thermocouple is connected with a temperature controller; the measuring lead is connected with the voltage measuring mechanism and the excitation lead is connected with the excitation signal source; according to the measuring device, the coil is wound in the groove of the ceramic sample box, even if the insulating layer on the outer layer of the coil is oxidized and falls off after multiple times of measurement, the phenomenon that the coil of adjacent turns is overlapped to generate short circuit can be avoided, so that the stability in the detection process is improved, and the accuracy of the detection result is ensured.
While the preferred embodiments of the present application have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all alterations and modifications as fall within the scope of the application.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present application without departing from the spirit and scope of the application. Thus, if such modifications and variations of the present application fall within the scope of the claims of the present application and their equivalents, the present application is intended to include such modifications and variations as well.
Claims (10)
1. A measuring device for curie temperature of a magnetic material, the measuring device comprising:
the heating furnace comprises a hearth;
the temperature controller is used for controlling the temperature of the heating furnace;
the surface is provided with a ceramic sample box with P circles of grooves; the ceramic sample box is placed in a temperature equalizing zone of the hearth after a sample to be detected is placed in the ceramic sample box, and P is more than or equal to 4;
the excitation lead is used for winding M turns of excitation coils in the groove of the ceramic sample box, wherein M is more than or equal to 2;
the measuring lead is used for winding N measuring coils in the groove of the ceramic sample box, wherein N is more than or equal to 2;
the thermocouple is used for measuring the temperature of the sample to be measured; the lead of the thermocouple is connected with the temperature controller;
the hollow connecting rod is arranged in the hearth and used for leading the excitation lead and the measurement lead out of the hearth;
the voltage measuring mechanism is connected with the measuring lead and is used for measuring the induced voltage of the sample to be measured;
and the excitation signal source is connected with the excitation lead wire and is used for providing excitation current in the measurement process.
2. The measurement device of claim 1, further comprising a data acquisition mechanism coupled to the temperature controller and the voltage measurement mechanism for acquiring temperature data and induced voltage data.
3. The measurement device according to claim 1, wherein the value of P is in the range of 24 to 30.
4. The measuring device of claim 1, wherein the ceramic sample cell is provided with a feedthrough.
5. The measurement device of claim 1, wherein the connecting rod is a ceramic connecting rod.
6. The measurement device of claim 1, wherein the ceramic sample cartridge is an annular sample cartridge.
7. The measuring device according to claim 6, wherein the ceramic sample case has an inner diameter of 12 to 16mm and an outer diameter of 26 to 34 mm.
8. A method for measuring the curie temperature of a magnetic material, wherein the measuring apparatus according to any one of claims 1 to 7 is used, and the method comprises:
placing a sample to be detected into the ceramic sample box, wherein the ceramic sample box is positioned in a uniform temperature zone of the hearth, M turns of excitation coils and N turns of measuring coils are wound on the ceramic sample box, and the thermocouple is arranged on the ceramic sample box;
determining a heating process and excitation parameters, controlling the heating furnace to heat up by the temperature controller according to the heating process, and outputting excitation current by the excitation signal source according to the excitation parameters;
acquiring temperature data and induction voltage data of the sample to be detected in the heating process;
and determining the Curie temperature of the sample to be detected according to the temperature data and the induced voltage data.
9. The method of claim 8, wherein determining the curie temperature of the sample to be measured from the temperature data and the induced voltage data comprises:
fitting by taking the temperature data as an X axis and the induced voltage data as a Y axis to obtain an induced voltage-temperature fitting curve;
solving a first derivative of the induction voltage-temperature fitting curve;
and determining the temperature value corresponding to the maximum value in the first-order derivative as the Curie temperature of the sample to be detected.
10. The measuring method according to claim 8, wherein if the sample to be measured is an annular forged material sample or a plate sample, the inner diameter of the sample to be measured is controlled to be not less than 18mm, the outer diameter of the sample to be measured is controlled to be not more than 24mm, and the total height of the sample to be measured is controlled to be not more than 10 mm;
and if the sample to be detected is a sheet sample, controlling the width of the sample to be detected to be less than 10mm and the thickness of the sample to be detected to be 5-10 mm.
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| CN114740039A (en) * | 2022-03-22 | 2022-07-12 | 首钢智新迁安电磁材料有限公司 | Strip steel temperature identification method and system, electronic equipment and storage medium |
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