CN104407007A - Method for determining melting temperature interval and melting behavior of metallurgical slag - Google Patents
Method for determining melting temperature interval and melting behavior of metallurgical slag Download PDFInfo
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- CN104407007A CN104407007A CN201410782800.3A CN201410782800A CN104407007A CN 104407007 A CN104407007 A CN 104407007A CN 201410782800 A CN201410782800 A CN 201410782800A CN 104407007 A CN104407007 A CN 104407007A
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Abstract
The invention provides a method for determining the melting temperature interval and the melting behavior of metallurgical slag and belongs to the technical field of detection of metallurgy materials. According to the method, a thermocouple has dual functions of directly heating a slag sample and directly measuring the temperature of the slag sample simultaneously, the specific melting temperature interval of the metallurgical slag sample is determined according to the characteristic that the slag sample needs to absorb heat during melting and the principle that an absorption peak is produced due to the fact that the slag sample temperature actually acquired by the thermocouple deviates from the target temperature of a set temperature rise curve, and then a characteristic video image, which is synchronously observed and recorded by an imaging system, of the change of the metallurgical slag during heating is intercepted so as to represent the specific change behavior of the metallurgical slag sample during melting in the time range corresponding to the determined melting temperature interval of the metallurgical slag sample. The method has the advantages that the method is simple and convenient to operate, measuring results are direct and accurate, the detection speed is high and the application range is wide, and the method can be used as a novel important detection means for accurately and effectively evaluating high-temperature characteristics of different metallurgical slag samples.
Description
Technical field
The invention belongs to metallurgical slag class material inspection technical field, in particular, provide a kind of method measuring metallurgical slag molten temperature region and melting behavior; Be applicable to the research as blast furnace slag, vessel slag, covering slag and other metallurgical class slag charges in field of metallurgy.
Background technology
In metallurgical process, require that slag has good metallurgical physical and chemical performance during smelting, such as blast furnace low temperature ironmaking technology requires that blast furnace slag is compared with having good mobility under low temperature, to realize carbon reduction; Electric furnace smelting requires that slag has good conductive capability, is conducive to selecting suitable power supply parameter, reduces power consumption; The claimed slag of high-speed continuous casting has lower temperature of fusion, to ensure enough supplies of melt cinder, produces the steel of high-quality.Therefore, slag high temperature physicochemical characteristic on metallurgical process carry out smoothly and the quality of product has important impact.
The hot properties of research slag carries out blending optimization to metal smelt, and has directive significance, so the hot properties of people to slag has carried out a large amount of work to the metallurgical reaction controlled in liquid steel-making, ironmaking processes.And for the mensuration of molten temperature region and melting behavior, be the primary prerequisite of the hot properties of research slag.Such as pneumatic steelmaking, if the temperature of fusion of slag is high, slag viscosity is too large, and dynamic conditions is bad, is unfavorable for the smelting (as dephosphorization, desulfurization etc.) of steel; On the contrary, the temperature of fusion of slag is low, the viscosity of slag is little, during blowing, slag seriously can wash away and corrode the serviceable life that furnace lining reduces furnace lining, thus, when working of a furnace condition is permitted, the temperature of fusion (temperature when so-called temperature of fusion refers to that solid matter changes homogeneous liquid phase completely into) of slag should be reduced as much as possible.Temperature of fusion both can be determined by phasor, also can measure by experiment, but due to the complicacy of actual slag components, existing Molten slag phase graph limited amount, and the overwhelming majority is low constituent element phasor, therefore generally can only be as a reference.In addition, the mensuration of slag melting is also more difficult because slag it and there is fixing fusing point unlike pure material, but the potpourri be made up of multiple compounds, its fusion process completes in a temperature range.
The assay method of usual slag molten temp can be summarized as two large classes: a class is the direct method of measurement, comprises molten steel Molten Slag Method and sample deformation method.So-called molten steel Molten Slag Method, namely slag is put on the long-pending molten steel of uniform temperature and certain surface in induction furnace, observe and record temperature corresponding when slag specimen starts to melt and melt completely, and determining burn-off rate by the time dependent relation of record slag layer thickness simultaneously.Although the method is close to the actual service condition of slag, the stability due to condition determination is too poor and cost of determination is too high, is difficult to application.Sample deformation method is that the relation by measuring sample deformation amount and temperature carries out characterizing, and the temperature that definition specimen height reduces to 1/2 of original height when being semisphere is hemisphere point temperature, i.e. the temperature of fusion of slag; Definition specimen height reduce to original height 1/4 in semisphere time temperature be the flow temperature of slag.This method comprises the slag melting characteristic determiner of LZ-III type, GXA type melting point apparatus and the full-automatic slag melting of RDS-04 and melts fast analyzer etc., all by adding warm sludge post in various heating furnace, the shape project of sample to screen will carry out the mensuration of slag hemisphere point temperature by optical system simultaneously, this method not only measuring accuracy is not high, and Measuring Time is long, efficiency is low; Another kind of is Indirect Determination, as: RTW-physical properties of melt comprehensive tester etc., it is the relation of the viscosity with temperature change by measuring slag specimen, drawing process is carried out again according to temperature-viscosity curve, thus obtain the melting temperature of slag specimen, in addition, the temperature of fusion adopting DTA or the DSC curve of differential thermal analyzer measurement slag in temperature-rise period to analyze slag specimen is also had.This class methods measuring accuracy is not high yet, and cannot observe the whole detailed process of slag specimen fusing.
Because the classic method measuring slag molten temp exists many deficiencies; at present; Chinese patent (application number is 200510046072.0) discloses a kind of assay method of fusion temp. of continuous casting protection slag; temperature of fusion is determined according to covering slag conductive voltage variation with temperature curve in fusion process; although the precision measured is compared hemisphere point method and improve, the concrete melting behavior of slag can not be observed real-time in-situ.Chinese patent (application number is 201110402527.3) discloses a kind of method of slag class material melting behavior and fusing point test, although this method adopts high temperature Laser Scanning Confocal Microscope, by Real Time Observation to slag class material fusing characteristic image characterize and reflect the melting behavior of slag class material and determine fusing point, although directly perceived, reliably, but it is harsh to slag class material dress sample process entails, and need constantly to adjust microscopical focal length when observing, in addition due to the existence of crucible medium, there is deviation in the temperature of fusion read and the actual temperature of fusion of slag specimen.Therefore, development research goes out a kind ofly actual temperature that directly Accurate Determining the is slag melting method that can observe again the concrete melting behavior of slag in whole process in real time to have extremely important effect and practical significance for the high temperature melting characteristic characterizing slag.
The maximum feature of thermocouple assay system is that it adopts directly heated sample can either directly measures the B type thermocouple of sample temperature as core parts again simultaneously.This system is made up of four parts such as B type thermocouple, imaging device, reaction chamber and central processing units, and wherein central processing unit comprises data collector and image recording structure.Form imaging device by CCD video capture device, microscope and tv display screen, be positioned at the top of reaction chamber, in order to imaging during high temperature is more clear, a filter is also housed at the top of reaction chamber, the strong infrared light of the part of sample when high temperature can be filtered out.The cavity that this reaction chamber adopts transparency silica glass to make, symmetria bilateralis is provided with two conduits, can airtightly also can open wide, curve U-shaped after B type thermocouple as heating temperature element be inserted in the conduit of reaction chamber, pass through heating control apparatus, namely PID temperature controller controls the heating rate of thermopair or rate of temperature fall heats or cools sample, the actual temperature of heated sample thermopair can be gathered by data collector, the modified-image of example reaction process can be observed and record by image recording structure, and can show on the tv screen in real time, in addition, experiment terminates rear temperature data and video file and can be stored in central processing unit and be convenient to call preservation.
This thermocouple assay system is mainly used in the crystallization behavior studying covering slag in continuous cast mold at present; comprise the crystallization behavior in continuous cooling process and the crystallization behavior in melting isothermal process; characterize the quality of covering slag crystal property with this, it is mainly that the video image collected by observation and analysis characterizes the design parameter of covering slag crystal property.Due to the complex system that the covering slag in continuous cast mold is made up of multiple compounds; its crystallization process is a nonequilibrium dynamic process; need to complete in a temperature range; be called FCTA temprature with the temperature started when there is crystal, be called crystallization final temperature with temperature when changing crystal completely into.As everyone knows, crystallization process is one becomes the solid-state process of regular arrangement by not too regularly arranged liquid phase, contrary with fusion process, although corresponding latent heat can be discharged along with the precipitation of crystal in the middle of this process, but first will forming core be there is in this process, relatively slow and tranquil, especially in isothermal crystal process, this situation is obvious especially, violent reaction can not be there is in it as fusion process, in addition, for continuous cooling process, the crystallization process impact of cooling rate on continuous casting covering slag is very large, when cooling rate is excessive, can not crystallize out, also have little time release latent heat and be just directly transformed into glass, even if the actual temperature of temperature thermocouple Real-time Collection protection slag specimen, FCTA temprature and the crystallization final temperature of slag clearly can not be judged according to chilling temperature curve, cause and cannot measure, when thus utilizing the crystallization behavior of covering slag in thermocouple assay systematic study continuous cast mold, it is all the crystal property parameter analyzing covering slag according to the video image of record, instead of characterized by the Temperature numerical that thermopair directly collects.
Although thermocouple assay system can measure the crystallization behavior of continuous casting covering slag, but form complex system because metallurgical slag is one by multiple compounds, there is essential distinction in its reaction carried out at fusion process and crystallization process, and be also completely not identical with the thermal effect of fusion process and crystallization process, at crystallization process, the essence of its thermal effect is a process discharging latent heat slowly; And fusion process is the process of a violent absorption heat.The crystallized product that crystallization process obtains simultaneously is no longer the single compound in original slag specimen composition, but the complex compound that in original slag specimen composition, the reaction of binary, ternary or even multicomponent mixture is formed.So fusion process is never the inverse process of crystallization process; Therefore can not be used as according to the FCTA temprature in crystallization process and termination Tc the molten temperature region judging covering slag simply.
In a word, up to the present, also nobody adopts thermocouple assay system to do detailed research to metallurgical slag molten temperature region and melting behavior.
Summary of the invention
The object of the present invention is to provide a kind of method measuring metallurgical slag molten temperature region and melting behavior, the method is with conspicuous characteristics, with the obvious advantage, and application prospect is extensive, can be that academic research and production actually provide reliably, theoretical foundation and technical support intuitively.
The present invention's thermocouple system used is made up of four parts such as B type thermocouple, imaging device, reaction chamber and central processing units, and wherein central processing unit comprises data collector and image recording structure.Form imaging device by CCD video capture device, microscope and tv display screen, be positioned at the top of reaction chamber, in order to imaging during high temperature is more clear, a filter is also housed at the top of reaction chamber, the strong infrared light of the part of sample when high temperature can be filtered out.The cavity that this reaction chamber adopts transparency silica glass to make, symmetria bilateralis is provided with two conduits, can airtightly also can open wide, curve U-shaped after B type thermocouple as heating temperature element be inserted in the conduit of reaction chamber, pass through heating control apparatus, namely PID temperature controller controls the heating rate of thermopair or rate of temperature fall heats or cools sample, the actual temperature of heated sample thermopair can be gathered by data collector, the modified-image of example reaction process can be observed and record by image recording structure, and can show on the tv screen in real time, in addition, experiment terminates rear temperature data and video file and can be stored in central processing unit and be convenient to call preservation.
A kind of method measuring metallurgical slag molten temperature region and melting behavior of the present invention, comprises the steps:
Step one
Adopt thermocouple assay system as detection system, and set the standard heating rate of thermocouple wire in thermocouple assay system; Described thermocouple assay system comprises thermocouple wire, imaging device, reaction chamber and central processing unit; Described middle central processing unit comprises data collector and image recording structure; Described imaging device is made up of video capture device, microscope and tv display screen; Described thermocouple wire is U-shaped thermocouple wire;
Step 2
Being loaded in by slag specimen to be measured on thermocouple wire is placed in reaction chamber, open imaging device and regulate microscopical focal length, until slag specimen to be measured clearly can be observed, then heat up by standard heating rate, and synchronous reading, the record actual temperature of thermocouple wire and the video image of slag specimen to be measured; When the actual temperature of thermocouple wire starts to depart from the target temperature corresponding to this moment standard heating rate, then think that the actual temperature of this moment thermocouple wire is the incipient melting temperature of slag to be measured, continue heating, when the actual temperature of thermocouple wire revert to the target temperature corresponding to this moment standard heating rate, then think that the actual temperature of this moment thermocouple wire is the complete temperature of fusion of slag to be measured; Then the concrete molten temperature region of slag specimen to be measured is determined according to the incipient melting temperature of slag specimen to be measured and complete temperature of fusion.
In actual application, target temperature corresponding to this standard heating rate and the graph of a relation of time can be prepared according to the standard heating rate of thermocouple wire.Time in this graph of a relation is synchronous with the heating-up time filled after sample.Namely the time in this graph of a relation carries out the time measured of heating up after being dress sample.
A kind of method measuring metallurgical slag molten temperature region and melting behavior of the present invention, described standard heating rate is 1 DEG C/min ~ 1800 DEG C/min, is preferably 800 DEG C/min ~ 1000 DEG C/min; More preferably 900 DEG C/min.
A kind of method measuring metallurgical slag molten temperature region and melting behavior of the present invention, slag specimen to be measured is glassy state slag specimen; Its particle diameter≤100 order.
The preparation method of described slag specimen to be measured is: by each component of slag specimen join get raw material after mix, then mixed-powder is placed in graphite crucible, heating is dissolved, and shrend after 1450 DEG C ~ 1600 DEG C heating and thermal insulation 8 ~ 15min, dry, broken, obtain particle diameter≤100 object slag specimen to be measured.
A kind of method measuring metallurgical slag molten temperature region and melting behavior of the present invention, described thermocouple wire is diameter 0.5mm, curves the U-shaped B type thermocouple that spacing is 2.5mm ~ 3.0mm.
A kind of method measuring metallurgical slag molten temperature region and melting behavior of the present invention, is loaded in slag specimen to be measured on the thermocouple wire of thermocouple assay system, is realized by following proposal:
After thermocouple wire being heated to 500 DEG C ~ 600 DEG C, by sticky mode of getting, slag specimen to be measured being attached on the U-shaped end of thermocouple wire, after then this thermopair being turned back to reaction chamber, the temperature of thermocouple wire and reaction chamber being down to room temperature.In actual mechanical process, be generally get about 5g slag specimen to be measured to be placed in surface plate, then the thermocouple wire of 500 DEG C ~ 600 DEG C be placed on slag specimen to be measured gently, rotate thermocouple wire, make it adhere to about 500mg slag specimen to be measured.
After the indoor thermocouple wire that slag specimen to be measured is housed of question response is down to room temperature, open imaging device and regulate microscopical focal length, until slag specimen to be measured clearly can be observed, then heat up by standard heating rate, and synchronous reading, the record actual temperature of thermocouple wire and the video image of slag specimen to be measured.
A kind of method measuring metallurgical slag molten temperature region and melting behavior of the present invention, the feature video image that in step 2, the melting behavior of slag specimen is captured by the inter-sync of intercepting molten temperature region characterizes, video image when described feature video image comprises incipient melting, in fusion process, in solid phase clusters image, fusion process, liquid phase wraps up the video image of solid phase, and video image when melting completely.
Principle and advantage
The present invention makes public for the first time and adopts thermocouple system to measure the method for metallurgical slag molten temperature region and melting behavior.Make use of thermopair directly heated sample can either directly can measure again the dual-use function of the actual temperature of sample simultaneously.By setting the standard heating rate of thermopair, and prepare the graph of a relation of target temperature and time according to this standard heating rate; It is simultaneously the test duration by timing definition in this graph of a relation cleverly, this makes, in testing process, can the be real-time actual temperature of thermopair and target temperature be contrasted, once find skew, can assert that this temperature is the incipient melting temperature of slag charge to be measured, in heating process subsequently, once find that the actual temperature of thermopair revert to target temperature, then can assert that this temperature is the complete temperature of fusion of slag charge to be measured.
On pretreatment, according to the actual situation of being heated of slag making raw material in production smelting process, heating rate choose reasonable when thermopair being heated slag specimen is set to 900 DEG C/min, and heating rate is too high or too small, and the result of mensuration is unfavorable for that Instructing manufacture is put into practice in the present invention.The output of electric thermo-couple temperature is controlled by heating control apparatus PID temperature controller, can can calculate target temperature corresponding to corresponding time point according to the standard heating rate of setting and minute thus, the data collector in addition in central processing unit can directly collect the actual temperature of heat hot galvanic couple and preserve simultaneously.Fusion process due to slag specimen is one and absorbs heat process clearly, so slag specimen can absorb heat from heat hot galvanic couple naturally when fusing, thus the actual temperature of the thermopair causing data collector to collect can lower than the target temperature arranged corresponding to heating rate, this situation meeting is until whole fusion process terminates, wherein incipient melting temperature starts lower than the target temperature arranged corresponding to heating rate as mark with the actual temperature collected, complete temperature of fusion just returns with the actual temperature collected and arranges target temperature corresponding to heating rate for mark, that is, Temperature numerical corresponding when determining that metallurgical slag is incipient melting and melt completely by the starting point of thermopair endothermic peak, accurately can obtain the molten temperature region of metallurgical slag specimen.In addition, because the present invention is when measuring, additionally use by CCD video capture device, the imaging device that microscope and tv display screen are formed, while collection slag specimen temperature data, the video image that slag specimen changes in heating process is saved by imaging device synchronous recording, it can catch the dynamic change of slag specimen in fusion process in real-time continuous ground, thus according to the time period corresponding within the scope of the above-mentioned molten temperature region determined, intercept synchronization acquistion to can reflect slag specimen from time incipient melting to the feature video image in the whole fusion process terminated when melting completely to characterize the concrete melting behavior of slag specimen, comprise metallurgical slag specimen incipient melting time characteristic image, characteristic image when melting completely, and in fusion process about the characteristic image changed between solid liquid phase.
Advantage of the present invention:
1. data are true, reliable.This method is when measuring molten temperature region and the melting behavior of slag specimen, because slag specimen directly contacts with thermopair, there is not other media or medium as crucible etc. in centre, the temperature of measurement is the actual temperature of slag specimen, than assay method in the past, result is more true, reliable.
2. result is vivid, directly perceived.This method is when measuring molten temperature region and the melting behavior of slag specimen, adopt video grabber, can in real time, original position, to observe and the dynamic melting behavior of record slag specimen in whole heating process online continuously, corresponding molten state can be characterized by intercepting synchronization video image, both image, directly perceived, very clear again.
3. simple, convenient.This method is when measuring molten temperature region and the melting behavior of slag specimen, the manually temperature of Schema control thermopair, directly carries out dry slag dress sample, requires harsh like that without the need to image height temperature Laser Scanning Confocal Microscope method, enormously simplify dress sample process, operate more convenient and practical.
4. detection speed is fast.This method is when measuring molten temperature region and the melting behavior of slag specimen, because heating rate is 900 DEG C/min, close to the actual conditions of slag charge fusing in smelting process, and adopt the mode of heating furnace heating to obtain many soon than traditional measurement method, the time measuring a slag specimen only needs the time of a few minutes, to substantially increase the speed of detection.
5. applied widely.This method is when measuring molten temperature region and the melting behavior of slag specimen; due to the platinum-rhodium alloy thermopair of the heating temperature element that adopts to be diameter the be B calibration of 0.5mm; maximum temperature can reach 1600 DEG C; far above the temperature of fusion of metallurgical slag class, thus this method can measure the molten temperature region and melting behavior that comprise blast furnace slag, molten iron pretreatment slag, vessel slag, covering slag and other metallurgical slag classes etc.
Accompanying drawing explanation
Accompanying drawing 1 is thermocouple assay system;
Accompanying drawing 2 is the preparation process schematic diagram of slag specimen;
The standard heating curve of accompanying drawing 3 set by embodiment 1 and reach the temperature lowering curve after design temperature;
Accompanying drawing 4 is the schematic diagram judging liquid iron pretreatment dephosphorizing slag molten temperature region in embodiment 1;
Accompanying drawing 5 is the schematic diagram characterizing liquid iron pretreatment dephosphorizing slag melting behavior in embodiment 1;
Accompanying drawing 6 is standard heating curve set in embodiment 2 and the temperature lowering curve after reaching design temperature;
Accompanying drawing 7 is the schematic diagram that embodiment 2 judges covering slag molten temperature region;
Accompanying drawing 8 is the schematic diagram characterizing embodiment 2 continuous casting covering slag melting behavior.
In Fig. 1,1 is imaging device, and 2 is reaction chamber, and 3 is U-shaped B type thermocouple, and 4 is heating control apparatus, and 5 is central processing unit, and 6 is filter, and 7 is conduit, and 8 is through hole.As can be seen from Figure 1 the composition of thermocouple assay system.
In Fig. 2, A1 is the potpourri of each component composition of slag specimen, and A2 is lapping device, and A3 is graphite crucible, and A4 is induction heater, and A5 is shrend container, and A6 is drying box, and A7 is surface plate.As can be seen from Figure 2, after joining each component of getting slag specimen by the component of design, tentatively grind, then load in graphite crucible after induction heater heating, shrend, drying, be ground to particle diameter≤100 order again, obtain slag specimen to be measured, then slag specimen to be measured is loaded in surface plate for subsequent use.
As can be seen from Figure 3 in embodiment 1, research liquid iron pretreatment dephosphorizing slag dissolve behavior time, the slope of the standard heating curve of its setting is 900 DEG C/min, after temperature reaches 1600 DEG C, lowers the temperature by the rate of temperature fall of 1800 DEG C/min.
There is deviation in the target temperature of the temperature and setting that obviously can observe thermopair actual measurement from Fig. 4, its value is lower than the target temperature arranged, this is because the fusion process of slag specimen is the process of a heat absorption, need to obtain heat from the external world, the temperature causing thermopair to record reduces.When the temperature of actual measurement and the target temperature of setting consistent time, show that slag specimen is fused into homogeneous liquid phase completely, no longer absorb heat.The incipient melting temperature of current measured liquid iron pretreatment dephosphorizing slag is 1417 DEG C, and complete temperature of fusion is 1501 DEG C, and namely molten temperature region is 1417 DEG C ~ 1501 DEG C.
As can be seen from Figure 5, in heating process, dephosphorized slag slag specimen does not almost significantly change below 1400 DEG C, when being raised to more than 1400 DEG C, slag specimen different parts successively starts to shrink to move, then near thermopair, there is liquid phase, along with the continuation of temperature raises, liquid phase is constantly expanded, solid phase generation clusters phenomenon, when solid phase be fused into gradually liquid phase reduce to a certain degree time, the solid phase of reuniting is by the complete moistening encirclement of liquid phase, then solid phase melts gradually and disappears until form the homogeneous phase liquid slag of melting, in the whole process of dephosphorized slag fusing, the solid phase observing reunion can be moved in fusion process, the phenomenons such as rotation, seldom observe in liquid phase the phenomenon having bubble formation.Constitutional diagram corresponding when what the A in current Fig. 5 intercepted is liquid iron pretreatment dephosphorizing slag incipient melting (namely temperature of fusion is 1417 DEG C), what the B in Fig. 5 intercepted is the constitutional diagram that liquid phase forms solid phase clusters, the solid phase of clusters that what C in Fig. 5 intercepted is by the constitutional diagram of the moistening encirclement of liquid phase, the constitutional diagram that what the D in Fig. 5 intercepted is when liquid iron pretreatment dephosphorizing slag melts completely (namely temperature of fusion is 1501 DEG C) when being the homogeneous phase liquid slag of melting.Wherein A → B → C → D reflects the exemplary dynamic behavior of liquid iron pretreatment dephosphorizing slag slag specimen in fusion process jointly.
As can be seen from Figure 6 in embodiment 2, research continuous casting covering slag dissolve behavior time, the slope of standard heating curve of its setting is 900 DEG C/min, after temperature reaches 1600 DEG C, lowers the temperature by the rate of temperature fall of 900 DEG C/min.
The Temperature numerical of thermopair actual measurement can be observed lower than the target temperature arranged from Fig. 7; this is melted by covering slag slag specimen and causes; because covering slag fusion process is the process of a heat absorption; need the external world to give heat could melt, the Temperature numerical causing thermopair to record thus is lower than the target temperature arranged.After fusing terminates, do not need to absorb heat again, the temperature of now thermocouple measurement is consistent with the target temperature of setting.The incipient melting temperature of current measured continuous casting covering slag is 1044 DEG C, and complete temperature of fusion is 1154 DEG C, and namely molten temperature region is 1044 DEG C ~ 1154 DEG C.
State when A reflection is incipient melting in Fig. 8, B reflects the phenomenon of fusion process solid phase clusters, and C reflects the phenomenon that reunion solid phase is wrapped up by liquid phase, and state when D reflection is melted completely, A → B → C → D reflects the melting behavior of continuous casting covering slag slag specimen jointly.As can be seen from Figure 8, in heating process, continuous casting covering slag slag specimen is substantially unchanged below 1000 DEG C, when being raised to more than 1000 DEG C, slag specimen near some position of thermopair starts to occur moving, along with the continuation of temperature raises, slag specimen starts drawdown deformation, then liquid phase is generated near thermopair place, now solid phase starts clusters phenomenon occurs, along with liquid phase is expanded gradually, the solid phase of reuniting is moved in fusion process, rotate, produce disappearance of breaking after much tiny bubble moves to rapidly surface in liquid phase simultaneously, compare liquid iron pretreatment dephosphorizing slag, the solidus melting speed of reuniting, arrive to a certain degree, wrapped up completely by liquid phase, then melt rapidly until disappear totally, show as continuous casting covering slag to melt completely.Constitutional diagram corresponding when what the A in current Fig. 8 intercepted is continuous casting covering slag incipient melting (namely temperature of fusion is 1044 DEG C); what the B in Fig. 8 intercepted is the constitutional diagram that continuous casting covering slag liquid phase forms solid phase clusters; the solid phase of continuous casting covering slag clusters that what C in Fig. 8 intercepted is is by the constitutional diagram of the moistening parcel of liquid phase, and what the D in Fig. 8 intercepted is when continuous casting covering slag melts (namely temperature of fusion is 1154 DEG C) is completely the constitutional diagram of single liquid phase.Wherein A → B → C → D reflects the exemplary dynamic behavior of continuous casting covering slag slag specimen in fusion process jointly.
Embodiment
Below in conjunction with example; select liquid iron pretreatment dephosphorizing slag slag specimen type different from continuous casting covering slag two kinds; by carrying out online the real time measure and observation to the molten temperature region of two kinds of slag specimens and melting behavior; be described in detail in temperature-rise period; the temperature of fusion of slag specimen from solid phase to the incipient melting temperature of liquid-phase conversion, when being transformed into homogeneous liquid phase completely, i.e. the dynamic behaviour of slag specimen fusing in molten temperature region and this process.
Embodiment 1
The Accurate Determining of liquid iron pretreatment dephosphorizing slag molten temperature region and the observation of melting behavior.
The present invention is applied in the mensuration of liquid iron pretreatment dephosphorizing slag molten temperature region and the observation of melting behavior, and concrete steps are as follows:
(1) prepare dephosphorized slag slag specimen: mixed in mortar by liquid iron pretreatment dephosphorizing slag slag charge and be placed on graphite crucible, be heated to about 1550 DEG C and melt and be incubated 10min and carry out shrend in induction furnace, after drying ,≤100 object powder slags are made in grinding.
(2) loading powder sample determination: manually pattern, thermopair is heated to about 580 DEG C, shake off sticky not steady powder slag after light sticky about 500mg dephosphorized slag slag specimen, and it is for subsequent use that this thermopair is turned back to reaction chamber, converts manual mode to automatic mode after temperature is dropped to room temperature; Then temperature rate and maximum temperature are set according to the temperature schedule (Fig. 3) in fusion process, open microscope and tv display screen simultaneously, by regulating microscopical focal length, until the slag specimen at thermopair tip clearly can be observed, start to add heat determination, and the synchronous video image capture device opened slag specimen temperature data acquisition device and change in heating process with record slag specimen, preserve stand-by after terminating in the lump.
(3) analysis temperature data: according to the historical temperature data of the direct heating dephosphorized slag thermopair that temperature data acquisition device collects, according to needing in material melts process to absorb heat thus the principle producing absorption peak carrys out the molten temperature region of Accurate Determining dephosphorized slag slag specimen.
(4) video image is processed: the video file terminating rear preservation by calling experiment, according to the result of slag specimen molten temperature region, intercept synchronization acquistion to can reflect slag specimen from time incipient melting to the feature video image in the whole fusion process terminated when melting completely to characterize the concrete melting behavior of dephosphorized slag slag specimen.
Main containing elements such as O, Ca, Si, Fe and P in the liquid iron pretreatment dephosphorizing slag of current employing, interpretation is as follows:
Fig. 4 is the schematic diagram judging liquid iron pretreatment dephosphorizing slag molten temperature region.There is deviation in the target temperature of the temperature and setting that obviously can observe thermopair actual measurement from Fig. 4, its value is lower than the target temperature arranged, this is because the fusion process of slag specimen is the process of a heat absorption, need to obtain heat from the external world, the temperature causing thermopair to record reduces.When the temperature of actual measurement and the target temperature of setting consistent time, show that slag specimen is fused into homogeneous liquid phase completely, no longer absorb heat.The incipient melting temperature of current measured liquid iron pretreatment dephosphorizing slag is 1417 DEG C, and complete temperature of fusion is 1501 DEG C, and namely molten temperature region is 1417 DEG C ~ 1501 DEG C.
Fig. 5 is the schematic diagram characterizing liquid iron pretreatment dephosphorizing slag melting behavior.In heating process, dephosphorized slag slag specimen does not almost significantly change below 1400 DEG C, when being raised to more than 1400 DEG C, slag specimen different parts successively starts to shrink to move, then near thermopair, there is liquid phase, along with the continuation of temperature raises, liquid phase is constantly expanded, solid phase generation clusters phenomenon, when solid phase be fused into gradually liquid phase reduce to a certain degree time, the solid phase of reuniting is by the complete moistening encirclement of liquid phase, then solid phase melts gradually and disappears until form the homogeneous phase liquid slag of melting, in the whole process of dephosphorized slag fusing, the solid phase observing reunion can be moved in fusion process, the phenomenons such as rotation, seldom observe in liquid phase the phenomenon having bubble formation.Constitutional diagram corresponding when what the A in current Fig. 5 intercepted is liquid iron pretreatment dephosphorizing slag incipient melting (namely temperature of fusion is 1417 DEG C), what the B in Fig. 5 intercepted is the constitutional diagram that liquid phase forms solid phase clusters, the solid phase of clusters that what C in Fig. 5 intercepted is by the constitutional diagram of the moistening encirclement of liquid phase, the constitutional diagram that what the D in Fig. 5 intercepted is when liquid iron pretreatment dephosphorizing slag melts completely (namely temperature of fusion is 1501 DEG C) when being the homogeneous phase liquid slag of melting.Wherein A → B → C → D reflects the exemplary dynamic behavior of liquid iron pretreatment dephosphorizing slag slag specimen in fusion process jointly.
Embodiment 2
The Accurate Determining in fusion temp. of continuous casting protection slag interval and the observation of melting behavior.
The present invention is applied in the mensuration in fusion temp. of continuous casting protection slag interval and the observation of melting behavior, and concrete steps are as follows:
(1) prepare covering slag slag specimen: mixed in mortar by continuous casting covering slag slag charge and be placed on graphite crucible, be heated to about 1500 DEG C and melt and be incubated 10min and carry out shrend in induction furnace, after drying ,≤100 object powder slags are made in grinding.
(2) powdered sample is equipped: manually pattern, thermopair is heated to about 520 DEG C, shake off sticky not steady powder slag after light sticky about 500mg covering slag slag specimen, and it is for subsequent use that this thermopair is turned back to reaction chamber, converts manual mode to automatic mode after temperature is dropped to room temperature; Then temperature rate and maximum temperature are set according to the temperature schedule (Fig. 6) in fusion process, open microscope and tv display screen simultaneously, by regulating microscopical focal length, until the slag specimen at thermopair tip clearly can be observed, start to add heat determination, and the synchronous video image capture device opened slag specimen temperature data acquisition device and change in heating process with record slag specimen, preserve stand-by after terminating in the lump.
(3) analysis temperature data: according to the historical temperature data of the direct heated protective slag thermopair that temperature data acquisition device collects, according to needing in material melts process to absorb heat thus the principle producing absorption peak carrys out the molten temperature region of Accurate Determining covering slag slag specimen.
(4) video image is processed: the video file terminating rear preservation by calling experiment; according to the result of slag specimen molten temperature region, intercept synchronization acquistion to can reflect slag specimen from time incipient melting to the feature video image in the whole fusion process terminated when melting completely to characterize the concrete melting behavior of covering slag slag specimen.
Main containing elements such as O, Ca, Al, Si, F and Na in current continuous casting covering slag, interpretation is as follows:
Fig. 7 is the schematic diagram judging fusion temp. of continuous casting protection slag interval.The Temperature numerical of thermopair actual measurement obviously can be observed lower than the target temperature arranged from Fig. 7; this is melted by covering slag slag specimen and causes; because covering slag fusion process is the process of a heat absorption; need the external world to give heat could melt, the Temperature numerical causing thermopair to record thus is lower than the target temperature arranged.After fusing terminates, do not need to absorb heat again, the temperature of now thermocouple measurement is consistent with the target temperature of setting.The incipient melting temperature of current measured continuous casting covering slag is 1044 DEG C, and complete temperature of fusion is 1154 DEG C, and namely molten temperature region is 1044 DEG C ~ 1154 DEG C.
Fig. 8 is the schematic diagram characterizing continuous casting covering slag melting behavior.In heating process, continuous casting covering slag slag specimen is substantially unchanged below 1000 DEG C, when being raised to more than 1000 DEG C, slag specimen near some position of thermopair starts to occur moving, along with the continuation of temperature raises, slag specimen starts drawdown deformation, then liquid phase is generated near thermopair place, now solid phase starts clusters phenomenon occurs, along with liquid phase is expanded gradually, the solid phase of reuniting is moved in fusion process, rotate, produce disappearance of breaking after much tiny bubble moves to rapidly surface in liquid phase simultaneously, compare liquid iron pretreatment dephosphorizing slag, the solidus melting speed of reuniting, arrive to a certain degree, wrapped up completely by liquid phase, then melt rapidly until disappear totally, show as continuous casting covering slag to melt completely.Constitutional diagram corresponding when what the A in current Fig. 8 intercepted is continuous casting covering slag incipient melting (namely temperature of fusion is 1044 DEG C); what the B in Fig. 8 intercepted is the constitutional diagram that continuous casting covering slag liquid phase forms solid phase clusters; the solid phase of continuous casting covering slag clusters that what C in Fig. 8 intercepted is is by the constitutional diagram of the moistening parcel of liquid phase, and what the D in Fig. 8 intercepted is when continuous casting covering slag melts (namely temperature of fusion is 1154 DEG C) is completely the constitutional diagram of single liquid phase.Wherein A → B → C → D reflects the exemplary dynamic behavior of continuous casting covering slag slag specimen in fusion process jointly.
Claims (8)
1. measure a method for metallurgical slag molten temperature region and melting behavior, it is characterized in that comprising the steps:
Step one
Adopt thermocouple assay system as detection system, and set the standard heating rate of thermocouple wire in thermocouple assay system; Described thermocouple assay system comprises thermocouple wire, imaging device, reaction chamber and central processing unit; Described middle central processing unit comprises data collector and image recording structure; Described imaging device is made up of video capture device, microscope and tv display screen; Described thermocouple wire is U-shaped thermocouple wire;
Step 2
Being loaded in by slag specimen to be measured on thermocouple wire is placed in reaction chamber, open imaging device and regulate microscopical focal length, until slag specimen to be measured clearly can be observed, then heat up by standard heating rate, and synchronous reading, the record actual temperature of thermocouple wire and the video image of slag specimen to be measured; When the actual temperature of thermocouple wire starts to depart from the target temperature corresponding to this moment standard heating rate, then think that the actual temperature of this moment thermocouple wire is the incipient melting temperature of slag to be measured, continue heating, when the actual temperature of thermocouple wire revert to the target temperature corresponding to this moment standard heating rate, then think that the actual temperature of this moment thermocouple wire is the complete temperature of fusion of slag to be measured; Then the concrete molten temperature region of slag specimen to be measured is determined according to the incipient melting temperature of slag specimen to be measured and complete temperature of fusion.
2. a kind of method measuring metallurgical slag molten temperature region and melting behavior according to claim 1, is characterized in that: described standard heating rate is 1 DEG C/and min ~ 1800 DEG C/min.
3. a kind of method measuring metallurgical slag molten temperature region and melting behavior according to claim 2, is characterized in that: described standard heating rate is 800 DEG C/and min ~ 1000 DEG C/min.
4. a kind of method measuring metallurgical slag molten temperature region and melting behavior according to claim 3, is characterized in that: described standard heating rate is 900 DEG C/min.
5. a kind of method measuring metallurgical slag molten temperature region and melting behavior according to claim 1, is characterized in that: slag specimen to be measured is dry glassy state slag specimen; Its particle diameter≤100 order.
6. a kind of method measuring metallurgical slag molten temperature region and melting behavior according to claim 1, is characterized in that: described thermocouple wire is diameter is 0.5mm, curve the U-shaped B type thermocouple that spacing is 2.5mm ~ 3.0mm.
7. a kind of method measuring metallurgical slag molten temperature region and melting behavior according to claim 1, is characterized in that: the maximum heating temperature of described thermocouple wire is 1600 DEG C.
8. a kind of method measuring metallurgical slag molten temperature region and melting behavior according to claim 1, it is characterized in that: the feature video image that in step 2, the melting behavior of slag specimen is captured by the inter-sync of intercepting molten temperature region characterizes, video image when described feature video image comprises incipient melting, in fusion process, in solid phase clusters image, fusion process, liquid phase wraps up the video image of solid phase, and video image when melting completely.
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