CN102162800B - Measuring device and method of crystallization temperature of crystallizer slag powder - Google Patents
Measuring device and method of crystallization temperature of crystallizer slag powder Download PDFInfo
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- CN102162800B CN102162800B CN2011100774649A CN201110077464A CN102162800B CN 102162800 B CN102162800 B CN 102162800B CN 2011100774649 A CN2011100774649 A CN 2011100774649A CN 201110077464 A CN201110077464 A CN 201110077464A CN 102162800 B CN102162800 B CN 102162800B
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Abstract
The invention relates to a measuring method for the crystallization temperature of crystallizer slag powder in the field of metallurgy, which is a simple and practical technology for measuring the crystallization temperature of slag powder. In the measuring device, a conductance method is adopted for measuring the crystallization temperature, and the measuring device is composed of a direct-current power supply U0, conductivity electrodes, a resistance furnace, a thermocouple, a digital-to-analog convertor, a data collector, a voltmeter and a protection resistor R0, wherein the temperature values of voltage and slag powder between two conductivity electrodes are synchronously collected by an external computer, and a corresponding relation schema is made, thus the crystallization temperature of the corresponding slag powder is obtained from the schema. Compared with the measuring method for the crystallization temperature of crystallizer slag powder, such as a differential thermal analysis method, a high temperature microscope method, a viscosity-temperature curve method and the like, the measuring method has the advantages of simple equipment, low cost, high precision and the like and is simple to operate.
Description
Technical field
The invention belongs to field of metallurgy, the measurement apparatus and method of more particularly to a kind of Crystalline Temperature of Mold Flux.
Background technology
Covering slag directly affects the direct motion of continuous casting and the surface quality of strand as functional material important in continuous casting, its metallurgical performance.Crystallization temperature, refers to that covering slag crystal in cooling procedure starts the temperature separated out, affects the distribution of slag film and structure between strand and crystallizer, be to coordinate heat transfer and the important parameter of lubrication.
The measurement topmost method of covering slag crystallization temperature has at present：Differential thermal analysis（DTA）, heating microscope method and viscosity-temperature curve method.Wherein DTA methods are the most commonly used, but for the less covering slag of some percent crystallization in massecuites, because crystallization liberated heat is few, differential thermal analysis balance can't detect exothermic peak, so that correct numerical value can not be read.Heating microscope method is directly observes, and the degree of accuracy is high, but equipment difficulty is sought, and cost is higher, is not suitable for general, substantial amounts of research.Viscosity-temperature curve method avoids direct measurement, using viscosity variation with temperature curve break as crystallization temperature, and cost is relatively low, but the value for generally believing measured by this method at present should be covering slag liquidus temperature and non-crystallization temperature.In summary, develop that a kind of to be suitable for numerous studies, the new covering slag crystallization temperature that measurement accuracy is high, cost is low detection means necessary.
The content of the invention
In order to solve the above problems, it is an object of the invention to provide a kind of measurement apparatus and method of the operation Crystalline Temperature of Mold Flux that relatively easy, cost is low, precision is high.
The technical scheme is that：A kind of measurement apparatus of Crystalline Temperature of Mold Flux, the device is by dc sourceU 0 , conductance electrode, resistance furnace, thermocouple, digital analog converter, data acquisition unit, voltmeter and protective resistanceR 0 Constitute；
Wherein, the conductance electrode is used for the magnitude of voltage for detecting covering slag to be measured；
The voltmeter set conductance electrode it is positive and negative on, the voltage for measuring the conductance electrode；
The dc sourceU 0 （For providing power supply for the conductance electrode；
The resistance furnace is used to place covering slag to be measured, and heats covering slag to be measured；
The installation of TC is in the bottom of the resistance furnace, the temperature value for gathering covering slag to be measured in real time；
The digital analog converter is connected with the voltmeter and the thermocouple respectively, for being changed to the data that the voltmeter and the thermocouple are collected, is sent to the data acquisition equipment；
The data acquisition unit is used for the data for receiving the digital analog converter conversion；
Protective resistanceR 0 The excessive damage circuit of electric current is prevented for protect whole circuit；The protective resistanceR 0 It is arranged onThe conductance electrode and the dc sourceU 0 Between.
Further, the device also includes lowering or hoisting gear, and the lowering or hoisting gear is made up of stepper motor, cantilever, electrode clamping device, support frame and leading screw.The progressive motor and the leading screw are installed on the bracket, and the cantilever is arranged on the leading screw, are moved up and down as described in the progressive motor drives edge leading screw, and the cantilever is provided with the electrode clamping device for being used for fixing the conductance electrode.
It is a further object of the present invention to provide the measuring method of the measurement apparatus of above-mentioned Crystalline Temperature of Mold Flux, following steps are specifically included：
Step by step rapid 2, the power supply for opening data acquisition unit simultaneously modulates program, then opens dc sourceU 0 , the voltage at two conductance electrode two ends of voltmeter measurementU, cooling is started with certain speed with the covering slag 3 in the seasonal molybdenum crucible, cooling rate is depending on slag system, and thermocouple gathers the temperature of the covering slag in the molybdenum crucible in real timeT, data acquisition unit by digital analog converter synchronously gather and record in real time；
Finally, according to the numerical value of record, with
For ordinate, with
For abscissa, the graph of a relation of the two is made, and finds the crystallization temperature of temperature, as covering slag corresponding when occurring discontinuous change in graph of a relation for the first time.
The measuring principle of the present invention is as follows：
Due to the resistance very little of conductance electrode, therefore the resistance of two conductance electrodes can be ignored, i.e.,R Electrode≈0Ω.Now, ifUFor the voltage between two conductance electrodes, then the relational expression of the voltage between electrical conductivity and two conductance electrodes can be obtained according to Ohm's law and the law of resistance：
Thus, the present invention just can beArrheniusLaw is converted to relational expression：
Above in all formulas, dFor electrode diameter；hFor the insertion depth of conductance electrode（Electrode base to covering slag liquid level distance）；lFor two electrode level intervals.
So, as long as recording voltage between two conductance electrodesUWith slag temperatureTThe change numerical value in covering slag cooling procedure, then withFor ordinate, with
For abscissa, the graph of a relation of the two is made, and finds temperature corresponding when occurring discontinuous change in graph of a relation for the first time, is the crystallization temperature for studying covering slag.
The beneficial effects of the invention are as follows：Measurement apparatus of the present invention is simple and easy to get, with low cost.Wherein, lowering or hoisting gear is made up of a set of step motor control system, a support frame and two cantilevers, by the rotating speed for setting stepper motor
Leading screw is driven, leading screw drives two cantilevers to move up and down again, meanwhile, a conductance electrode is fixed through clamping device in the end of every cantilever, them is not in contact with each other and all keeps vertical state.
Measuring method involved in the present invention, only need to connect measurement apparatus, modulate equipment and program, set rate of temperature fall, and after using lowering or hoisting gear, two conductance electrodes are inserted in covering slags, it is possible to gather the temperature of covering slag in real time using computerTVoltage between two conductance electrodesUChange, it is simple to operate.Empirical tests, compared with the measuring method of other existing covering slag crystallization temperatures, such as differential thermal analysis（DTA）, heating microscope method and viscosity-temperature curve method etc., measuring method of the invention is simple to operate, with low cost, accuracy is high.
4th, illustrate
Fig. 1 is a kind of measurement apparatus principle schematic of Crystalline Temperature of Mold Flux of the invention.
Fig. 2 is the structural representation of lowering or hoisting gear.
Fig. 3 is that the present invention measures two kinds of different slag systems in laboratory conditions
With
Graph of a relation.
In figure：
1 dc sourceU 0 ；2 conductance electrodes；3 covering slags；4 resistance furnaces；5 thermocouples；6 digital analog converters；7 data acquisition units；8 voltmeters；9 protective resistancesR 0 ；10 stepper motors；11 cantilevers；12 electrode clamping devices；13 support frames；14 leading screws.
Embodiment
Measuring method involved in the present invention will be described further by the elaboration to embodiment, and with reference to accompanying drawing below.
Fig. 1 is the measuring principle schematic diagram involved by the inventive method.As shown in figure 1, the device includes dc sourceU 0 1st, conductance electrode 2, resistance furnace 4, thermocouple 5, digital analog converter 6, data acquisition unit 7 and voltmeter 8.Dc sourceU 0 1Both positive and negative polarity be connected respectively with two identical conductance electrodes 2, from positive pole draw wire be provided with protective resistanceR 0 9；The positive pole of voltmeter is connect to the conductance electrode of positive pole, negative pole connects the conductance electrode of negative pole, i.e. what voltmeter was measured is the voltage between two conductance electrodes, and the digital analog converter 6 of voltmeter 8 is connected with data acquisition unit 7, the voltage between two conductance electrodes is gathered in real time so as to realize；The bottom of resistance furnace 4 is provided with thermocouple 5, and thermocouple 5 is connected by digital analog converter 6 with data acquisition unit 7, so as to realize the real-time collection to covering slag temperature.
Fig. 2 is the lowering or hoisting gear of conductance electrode, and this device includes stepper motor 10, support frame 14 and two steel cantilevers 11 being hinged on support frame；Two steel cantilever 11 is equipped with electrode clamping device 12, for two conductance electrodes are fixed on lowering or hoisting gear.Clamping device is wooden into fastening and insulation function, two conductance electrodes being made to be parallel to each other and keep vertical state, the insulation of conductance electrode and steel cantilever can be made again by insulating.Two conductance electrode materials are long 500mm, diameter 4mm MoSi2Rod.
If covering slag is considered as into oxide slag system, the conductivity variations feature under liquid phase state meetsArrheniusLaw, i.e.,：
In formula,κFor covering slag electrical conductivity, Ω-1·cm-1；AFor experimental constant, Ω-1·cm-1；RIt is gas constant, 8.314 JK-1·mol-1；TIt is absolute temperature, K；BFor conductivity activation energy, Jmol-1。
The analysis of above formula have ignored the structure variation with temperature of melt cinder, so that
WithLinear, slope is.And when there is crystal precipitation in liquid slag, B values will change, now
Due to B change and with
The linear relationship of script is no longer followed, and the jump of discontinuous change occurs, therefore can be by measuring electrical conductivity variation with temperature, so as to draw the crystallization temperature of covering slag.The measuring method of present invention temperature value corresponding when will appear from the first discontinuous change of B values is considered as the crystallization temperature of covering slag.
The specific implementation step of measuring method of the present invention is as described below：
Step 2, open the power supply of data acquisition unit 6 and modulate program, then open dc sourceU 0 1, voltmeter 8 measures the voltage at two two ends of conductance electrode 2U, cooling is started with certain speed with the covering slag 3 in the seasonal molybdenum crucible, cooling rate is depending on slag system, and thermocouple 6 gathers the temperature of the covering slag in the molybdenum crucible in real timeT, data acquisition unit 7 gathers and records in real time by the way that digital analog converter 6 is synchronous；
Finally, according to the numerical value of record, with
For ordinate, with
For abscissa, the graph of a relation of the two is made, and finds the crystallization temperature of temperature, as covering slag corresponding when occurring discontinuous change in graph of a relation for the first time.
Fig. 3 be implementation process of the present invention in, by two kinds difference slag systems measured, and with
For ordinate, with
The graph of a relation made for abscissa.As can clearly see from the figure, slag system 1 occurs in that obvious jumping characteristic change at 1050 DEG C for the first time, and slag system 2 occurs in that obvious jumping characteristic change at 1200 DEG C for the first time, therefore according to the measuring method of the present invention, the crystallization temperature of slag system 1 is 1050 DEG C, and the crystallization temperature of slag system 2 is 1200 DEG C.Empirical tests, compared with the measuring method of other existing covering slag crystallization temperatures, measuring method of the invention is simple to operate, with low cost, accuracy is high.
Specific embodiment
The method according to the invention, under laboratory conditions, the two kind protection slag systems different to composition are measured, and main component is shown in Table 1.Table 2 by the present invention and differential thermal analysis (DTA) and viscosity-temperature curve method to two kinds of slag system crystallization temperatures of research measurement result contrast verification.The voltage of dc source used in the present embodimentU 0 =8V；Protective resistanceR 0 =10Ω。
The main component of 1 two kinds of covering slags of table（%）
| Covering slag | Al2O3 | MgO | Na2O | F- | Li2O |
 |
Fusion |
| Slag | |||||||
| 1 | 3.00 | 3.81 | 7.34 | 8.83 | 0.79 | 1.19 | 1075℃ |
| Slag 2 | 2.54 | 1.02 | 8.34 | 8.87 | 3.0 | 1.4 | 1023℃ |
Note：
The contrast of the present invention of table 2 and differential thermal analysis and viscosity-temperature curve method measurement result
Empirical tests, compared with the measuring method of other existing covering slag crystallization temperatures, such as differential thermal analysis（DTA）, heating microscope method and viscosity-temperature curve method etc., measuring method of the invention is simple to operate, with low cost, accuracy is high.
Claims (1)
1. a kind of measuring method of the measurement apparatus of Crystalline Temperature of Mold Flux, the device is by dc sourceU 0 （1）, conductance electrode（2）, resistance furnace（4）, thermocouple（5）, analog-digital converter（6）, data acquisition unit（7）, voltmeter（8）And protective resistanceR 0 （9）Constitute；
Wherein, the conductance electrode（2）Magnitude of voltage for detecting covering slag to be measured；
The voltmeter（8）Conductance electrode is set（2）It is positive and negative on, the voltage for measuring the conductance electrode；
The dc sourceU 0 （1）For for the conductance electrode（2）Power supply is provided；
The resistance furnace（4）For placing covering slag to be measured, and heat covering slag to be measured；
The thermocouple（5）Installed in the resistance furnace（4）Bottom, the temperature value for gathering covering slag to be measured in real time；
The analog-digital converter（6）Respectively with the voltmeter（8）With the thermocouple（5）Connection, for the voltmeter（8）With the thermocouple（5）The data collected are changed, and are sent to the data acquisition unit（7）；
The data acquisition unit（7）For receiving the analog-digital converter（6）The data of conversion；
Protective resistanceR 0 （9）The excessive damage circuit of electric current is prevented for protect whole circuit；The protective resistanceR 0 （9）It is arranged onThe conductance electrode（2）With the dc sourceU 0 （1）Between；The device also includes lowering or hoisting gear, and the lowering or hoisting gear is by stepper motor（10）, cantilever（11）, electrode clamping device（12）, support frame（13）And leading screw（14）Composition；
The stepper motor（10）With the leading screw（14）Installed in support frame as described above（13）On, the cantilever（11）Installed in the leading screw（14）On, by the stepper motor（10）Drive the cantilever（11）Along the leading screw（14）Move up and down, the cantilever（11）Being provided with is used to fix the conductance electrode（2）Electrode clamping device（12）；Characterized in that, the measuring method specifically includes following steps：
Step 1; it will be contained in after covering slag carbonization treatment to be measured in molybdenum crucible; and put it into be connected with argon gas protection resistance furnace in be slowly heated more than fusion temperature; and slag to be protected is completely melt constant temperature for a period of time; two conductance electrodes are inserted vertically into liquid covering slag with a fixed speed; its insertion depth is depending on the height of crucible used, and insertion process should not touch crucible wall and bottom；
Step 2, open the power supply of data acquisition unit and modulate program, then open dc sourceU 0 , voltage
Table measures the voltage at two conductance electrode two endsU, cooling is started with certain speed with the covering slag in the seasonal molybdenum crucible, cooling rate is depending on slag system, and thermocouple gathers the temperature of the covering slag in the molybdenum crucible in real timeT, data acquisition unit by analog-digital converter synchronously gather and record in real time；
Finally, according to the numerical value of record, with
For ordinate, with
For abscissa, the graph of a relation of the two is made, and finds the crystallization temperature of temperature, as covering slag corresponding when occurring discontinuous change in graph of a relation for the first time.
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| CN2011100774649A CN102162800B (en) | 2011-03-29 | 2011-03-29 | Measuring device and method of crystallization temperature of crystallizer slag powder |
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| CN102520001B (en) * | 2011-12-06 | 2013-08-14 | 首钢总公司 | Crystallization behavior of slag material and determination method of crystallization temperature |
| CN102661967A (en) * | 2012-04-26 | 2012-09-12 | 中南大学 | Heat flow simulation test device of crystallizer meniscus horizontal heat transfer |
| CN102717040A (en) * | 2012-06-11 | 2012-10-10 | 内蒙古包钢钢联股份有限公司 | Measurement method for temperature protection of continuous casting tundish covering agent |
| CN103969292B (en) * | 2014-05-29 | 2016-04-20 | 中南大学 | A kind of continuous crystallizer protecting slag complex heat transfer heat flux measurement device and method |
| CN104407007A (en) * | 2014-12-16 | 2015-03-11 | 中南大学 | Method for determining melting temperature interval and melting behavior of metallurgical slag |
| CN104502222B (en) * | 2014-12-17 | 2017-04-26 | 大连理工大学 | Method for determining metastable region of high-concentration and low-light-transmittance solution system based on microporous membrane response |
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| KR20010058258A (en) * | 1999-12-27 | 2001-07-05 | 이구택 | Apparatus for evaluating the crystallization characteristics of mold flux |
| CN1657890A (en) * | 2005-03-22 | 2005-08-24 | 东北大学 | Measuring method and device for fusion temp. of continuous casting protection slag |
| CN101666614B (en) * | 2009-10-20 | 2011-08-10 | 北京科技大学 | Device and method for measuring thickness of molten slag layer of mold flux of continuous casting crystallizer |
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