CN102495096A - Method for determining melting behavior and melting point of slag-like material - Google Patents
Method for determining melting behavior and melting point of slag-like material Download PDFInfo
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Abstract
The invention relates to a method for determining a melting behavior and a melting point of a slag-like material, belonging to the technical field of detection of metallurgical slag-like material. The process comprises slag sample preparation, slag sample formation, high-temperature laser sample filling, experimental parameter setting, melting process observation and data and image processing. The method provided by the invention has the advantages that the defect of low accuracy of the slag column deformation method, i.e. the hemisphere point temperature testing method, in the traditional melting point testing can be overcome, and the limitations of difficulties in control of the stability of testing conditions and high testing costs in the method of slag melting in liquid steel can be eliminated. The initial melting temperature of the slag sample from the solid phase to the liquid phase and the melting temperature of the slag sample to the full liquid phase can be captured promptly so as to accurately determine the melting point of the slag sample; and the liquid phase nucleation, growth and other melting changes and behaviors of the slag sample in the heating process can also be analyzed, the direct theoretical basis and technical support can be provided for the curing of liquid slag and the control of metallurgical reaction in the steel-making and iron-making process, and different characteristics of different slag samples in the melting process can be used as an important means for evaluation of high-temperature properties of different slag samples.
Description
Technical field
The invention belongs to metallurgical slag class material tests technical field, the method for a kind of slag class material melts behavior and fusing point test particularly is provided; Be applicable to the research of blast furnace slag, covering slag and other slag charge.
Background technology
Smelting process requires slag to have good flowability; High-speed continuous casting requires covering slag to have low temperature of fusion; With enough supplies of assurance melt cinder, and the temperature of fusion of slag also has big meaning to the power supply parameter of selecting electric furnace smelting to guarantee suitable slag temperature and lower power consumption.Therefore, the temperature of fusion of slag has determined the temperature schedule in the metallurgical engineering, if the temperature of fusion of slag is high, slag viscosity is excessive, and is then unfavorable to the smelting and the desulfurization of steel; If the temperature of fusion of slag is low, slag viscosity is too low again, and slag can seriously wash away the erosion furnace lining and reduce lining durability during blowing.Consider energy-conservation, as to reduce fire resistive material and furnace lining factors such as loss, under the condition that the working of a furnace allows, require alap temperature of fusion usually.
It is thus clear that the temperature of fusion of rationally controlling slag has significance to the smelting of steel and the raising of lining durability.Therefore, the high-temperature behavior of slag and melting behavior are paid close attention to by numerous researcher.In recent years; Hot properties (fusing point, viscosity, component activity etc.) through the research slag is to the metal smelt optimization of preparing burden; The purpose that liquid towards is made steel in the hope of reaching, ironmaking processes control metallurgical reaction has directive significance; And for the accurate mensuration of fusing point, be the primary prerequisite of the hot properties of research slag, the cured that also can be slag provides the important theory reference.
Temperature of fusion is meant the temperature when solid matter is transformed into even liquid phase fully.Temperature of fusion can be confirmed through liquidus curve, liquidus surface or the isothermal temperature of melt phasor, also can obtain through measuring.The fusing point of slag is the liquidus temperature of this component on the slag state figure, but because melt temperature is high and the complicacy of actual slag system, general slag phasor can only be as a reference.In addition, the mensuration of slag melting is more complicated also, because the potpourri that slag is made up of multiple compound, it has fixing fusing point unlike pure material, and its fusion process is carried out in a temperature range.
At present; Research method to the fusing point test of slag is many, can reduce two types, and one type main measures the relation of sample deformation amount and temperature through using the sample deformation method; Temperature when specimen height is reduced to 1/2 of former height and is semisphere is decided to be hemisphere point temperature, promptly gets the temperature of fusion of slag; 1/4 o'clock hemispherical temperature (sample all becomes liquid state) of specimen height being reduced to former height is decided to be flow temperature.Its method of testing comprises slag post deformation method and various thermal characteristics appearance determination methods etc.Another kind of is molten steel slag method; Promptly in induction furnace; Slag is put on the long-pending molten steel of uniform temperature and certain surface, observed and the record slag begins to melt and the corresponding temperature of fusing fully, and can measure burn-off rate through slag layer thickness in the record unit time.This method of testing is near the service condition of slag in actual production, but the stability of condition determination is difficult to control, and cost of determination is high, and the popularization in actual production is restricted.
Owing in actual production, usually only need to understand the factor that slag becomes the temperature can working fluid the time and influences this temperature, it is comparatively general therefore to adopt semiempirical slag post deformation method to be that hemisphere point temperature is similar to the melting temperature of definite slag melting or slag.Wherein, In most thermal characteristics appearance determination methods, all adopt hemisphere point hygrometry like LZ-III type slag pre-arcing characterisitics analyzer, GXA type fusing point appearance, RTW-physical properties of melt comprehensive tester, SJY-1700 type image-type sintered point tester, the molten fast analyzer of the full-automatic slag melting of RDS-04 and RD505 MELTING POINT etc.; In addition, horizontal molybdenum wire furnace, SiC tubular furnace, molybdenum disilicide high temperature furnace and high-temperature tubular resistance furnace etc. also all are to project to specimen shape on the screen by optical system, carry out slag hemisphere point and measure; It is to analyze its temperature of fusion through measuring slag charge DTA or DSC curve in temperature-rise period that differential thermal analyzer is only arranged.Yet; No matter which kind of utilizes the thermal characteristics appearance determination method of hemisphere point temperature measuring slag melting, can only be similar to definite slag melting, and in practical operation, all have certain limitation; And utilize differential thermal analyzer to measure fusing point; Also can only qualitatively judge the fusing point of slag through the endothermic peak on DTA or the DSC curve, accuracy is limited, and the more important thing is that the melting behavior of slag can't realize dynamic observing.For this reason, development research goes out method of testing ten minutes necessity of the actual working state that can better reflect slag.
The high-temperature heater of high temperature confocal laser microscope adopts infrared lamp to focus on heating, and shaft is the hermetically-sealed construction of oval gold-plated minute surface, adopts computer-controlled program intensification and platinum-rhodium alloy thermopair to carry out thermometric.Its optical system object-image conjugate; Have only the point on the focal plane of lens could form the dot pattern picture through the pin hole spatial filtering; When two-forty scanning obtains high quality graphic, the heat damage of sample is reduced to minimum, also provide the slow scanning function to improve sensitivity simultaneously.In addition, LASER Light Source monochromaticity is good, and depth of focus is little after the imaging and focusing, and longitudinal frame is high, can nondestructively make the layer scanning and the fluorescence intensity measurement of different depth to sample, and the optical section of different focal planes obtains the 3-D solid structure of sample behind three-dimensional reconstruction.Therefore, can realize that material changes into the initial temperature of fusion of liquid phase and the in-situ dynamic observation that is completed into the temperature of fusion of liquid phase from solid phase in temperature-rise period.It is thus clear that, not only can accurately measure the fusing point of slag by the high temperature confocal laser microscope, and can the initial liquid phase of slag in the pyroprocess be generated, and liquid phase how forming core, fusion variation behavior such as grow up are analyzed and researched.
Yet, because most slags does not have metallic luster, can't form images at microscopically, can't observe the pattern of slag at all, also just can't further observe its melting behavior.Therefore, the sample preparation of slag is a primary difficult problem that solves.For this reason, the sample preparation and the observation of slag class sample have been carried out constantly groping and improving.Mainly contain following method:
(1) pad platinum sheet in crucible.Make full use of the metallic luster of platinum sheet, the pattern that places slag on the platinum sheet is seted off by contrast out.This method advantage is that the color and luster contrast is big, can clearly see the profile of slag.But shortcoming is that granular slag is vacuumizing or logical Ar
2During air-flow, because light weight body circle, roll easily and disperse distributes and blocks platinum sheet contrast, obviously reduce and observe sharpness, and the very tiny slag particle of granularity even possibly detached the platinum sheet is unfavorable to equipment.
(2) in view of the drawback of method (1), by viscosity apparatus with the slag of disperse shape through the bonding column that is fired into of dextrin.This method advantage is to vacuumize or logical Ar
2The time, can not block platinum sheet contrast, can observe the initial temperature of fusion of slag.But the slag column volume is bigger, in heating process, and difficult fusing that temperature is on the low side; The slag that temperature is higher then to cause molten state to around spread slime flux, very soon monoblock platinum sheet is all blocked, lose the observation contrast; Can't accurately observe the complete temperature of fusion of slag, and the crystallization behavior of temperature-fall period.
(3) in view of the drawback of method (2), the slag post is broken into fragment observes.Its advantage is to realize the initial temperature of fusion of slag and the mensuration of complete temperature of fusion, has broken through the successful mensuration of slag class sample fusing point under high temperature laser microscope first.But the glassy state slag specimen through fusion and cooling fast all is difficult for peeling off with crucible or platinum sheet, not only wastes crucible and platinum sheet, and main is to observe follow-up crystallization behavior.
(4) to the drawback of method (3); Adopt platinum or graphite crucible to prepare the glassy state slag; To avoid can't peeling off the waste that causes with crucible or platinum sheet after the slag specimen fusing, the fragment after fragmentation directly carries out the fusing point test, but follow-up crystallization behavior still can't be observed.Show through experiment repeatedly, the uneven components of glassy state slag be cause can't clear seizure crystallization behavior main cause.Finally by the opened type high temperature furnace, stir in heating process, and with gained glassy state slag through broken, grind to form ground-slag and carry out the fusing point test test.Not only the observation of melting behavior is more clear; The result is more accurate; And, can realize the clear observation of crystallization behavior through method improvement (concrete innovative approach sees that patent-a kind of research slag charge is in temperature-fall period crystallization behavior and the accurate method for measuring of crystallization point).
It is thus clear that the successful preparation of glassy state slag is only the condition precedent of the fusing point and the crystallization point of accurate mensuration slag.
Summary of the invention
The object of the present invention is to provide the method for a kind of slag class material melts behavior and fusing point test; But not only original position, continuously, melting behavior such as dynamic type observes the liquid phase forming core of slag in whole temperature-rise period, grow up, and can judge accurately that slag charge changes into the initial temperature of fusion of liquid phase and the temperature of fusion that is completed into liquid phase from solid phase.
The present invention has overcome traditional fusing point method of testing only through slag post deformation method (hemisphere point thermometry) the not high deficiency of accuracy; And the limitation that molten steel slag method condition determination stability is difficult to control, cost of determination is high; And test process is dynamically directly perceived, test result is accurate, thereby has traditional test method incomparable advantage and application prospect.
The present invention adopts high-temperature laser Laser Scanning Confocal Microscope original position, continuous, dynamic type observation slag melting behavior in whole temperature-rise period; Having overcome traditional fusing point method of testing is the not high deficiency of hemisphere point thermometry accuracy through slag post deformation method only, and the limitation that molten steel slag method condition determination stability is difficult to control, cost of determination is high.Not only can catch slag specimen in real time and change into the initial temperature of fusion of liquid phase and the temperature of fusion that is completed into liquid phase, realize the accurate mensuration of slag specimen fusing point from solid phase; The slag specimen of also can analyzing and researching changes behavior in temperature-rise period liquid phase forming core, fusion such as grow up; For the cured and the control of liquid steel slag are made steel, the metallurgical reaction of ironmaking processes provides theoretical foundation and technical support intuitively; And the different characteristic that in melting process, appeared of different slag specimens, can be used as the important means of estimating different slag specimen hot properties.Processing step is following:
1. slag specimen preparation: slag charge is placed platinum/graphite crucible, in opened type agitating heating stove, carry out high temperature (1400～1550 ℃) calcination, behind calcination to the glassy state slag, shrend.Again with cooled slag specimen through the disintegrating apparatus fragmentation after, with agate mortar fully grind, mixing processes 50～200 purpose ground-slags.
2. slag specimen moulding: by dextrin that powder appearance is bonding, and with anhydrous filter paper the ground-slag applying light is fixed on 3mm * 3mm platinum sheet, make the slag specimen moulding.
3. high-temperature laser is adorned appearance: the platinum sheet that the moulding slag specimen will be housed places the Al of Φ 8mm * 4mm
2O
3The bottom of crucible is again with Al
2O
3Crucible is put into high temperature (100～1700 ℃) the metallographic heating furnace of laser confocal microscope.
4. experiment parameter setting: will place the slag specimen of metallographic heating furnace to carry out vacuum pumping earlier, and set different intensification experimental arrangements (heating rate is 60～600 ℃/s, and the intensification temperature is 1300～1600 ℃) according to different slag class materials again, then at Ar
2Experiment heats up under the atmosphere protection.
5. fusion process is observed: can carry out Real Time Observation to fusion process through computer, and synchronous acquisition needs in the observation process to focus on adjustment at any time based on the definition of image to the dynamic menu of whole fusion process.Wherein, the initial temperature of fusion of slag specimen raises with temperature to observe solid-state slag specimen that to begin to occur vacuole be the sign (see figure 4).Slag specimen is completed into the temperature of fusion of liquid phase and sharply shrinks to observe solid-liquid coexistence slag specimen surface, has only liquid slag to exist for the sign (see figure 8) until being converted into fully.
6. data and Flame Image Process: after experiment finishes, preserve experimental data and results for video, the initial temperature of fusion of intercepting and be completed into the temperature of fusion of liquid phase corresponding typical picture and liquid phase forming core, fusion such as grow up changes the behavior video and analyzes.
Innovative point of the present invention is, one of which, but original position, continuously, how dynamic type observe slag from the solid-state whole process that transforms to liquid state, for the analysis and research slag specimen provides theoretical foundation in temperature-rise period liquid phase forming core, fusion variation behavior such as grow up; Its two, can catch slag specimen in real time and change into the initial temperature of fusion of liquid phase and the temperature of fusion that is completed into liquid phase from solid phase, realize the accurate mensuration of slag specimen fusing point.
Difficult point of the present invention that is technological innovation at first are the sample preparation of different slag charges is groped and successful sample preparation; Secondly; To the method improvements such as diffusing particle removing around pad selection, the processing of glassy state ground-slag, powder appearance forming processes and the agglomerate, grope; Also being the liquid phase forming core of finally successfully realizing clear observation slag under the different method for making sample, grow up etc., fusion changes the behavior and the key point of the accurate mensuration of slag specimen fusing point.
The invention has the beneficial effects as follows; It is the not high deficiency of hemisphere point thermometry accuracy through slag post deformation method only that this invention has overcome traditional fusing point method of testing; And the limitation that molten steel slag method condition determination stability is difficult to control, cost of determination is high; The cured that can be iron and steel enterprise's liquid steel slag provides theoretical foundation intuitively, with acquisition high activity solid steel slag, thus the level of resources utilization that improves steel manufacture process; The metallurgical reaction that also can be the steel-making of control liquid state, ironmaking actual production process provides relevant and instructs and technical support, also can be evaluation slag high-temperature behavior reference frame is provided.
Description of drawings
Below in conjunction with accompanying drawing and application example patent of the present invention is further specified.
Fig. 1 observes sample preparation process flow diagram before for slag charge.Wherein, slag charge 1, platinum/graphite crucible 2, opened type agitating heating stove 3, disintegrating machine 4, agate mortar 5, platinum sheet 6, Al
2O
3Crucible 7, high-temperature laser Laser Scanning Confocal Microscope 8.
Fig. 2 is the synoptic diagram of blast furnace slag in the melting process temperature schedule.
Fig. 3 is the temperature program synoptic diagram of covering slag at temperature-rise period.
Fig. 4 begins to generate the synoptic diagram (synoptic diagram of vacuole appears in the slag specimen surface) of temperature for judging slag specimen (is example with the blast furnace slag) liquid phase.
Fig. 5 begins to generate the synoptic diagram of temperature (vacuole increases and begin the synoptic diagram of group bunch) for judging slag specimen (is example with the blast furnace slag) liquid phase.
Fig. 6 is a slag specimen (is example with the blast furnace slag) at temperature-rise period liquid phase forming core, melting behavior synoptic diagram (synoptic diagram that liquid phase begins continuous forming core and grows up) such as grow up.
Fig. 7 is a slag specimen (is example with the blast furnace slag) in temperature-rise period liquid phase forming core, melting behavior synoptic diagram such as grow up (liquid phase continue increase, grow up synoptic diagram).
Fig. 8 melts the synoptic diagram (slag specimen is molten fully to be liquid synoptic diagram) that forms liquidus temperature fully for judging slag specimen (is example with the blast furnace slag).
Fig. 9 melts the synoptic diagram (slag specimen is molten fully to be the synoptic diagram that liquid back liquid phase is no longer grown up) that forms liquidus temperature fully for judging slag specimen (is example with the blast furnace slag).
Figure 10 is for judging slag specimen (is example with the covering slag) liquid phase and begin to generate and the synoptic diagram (the apparent shape appearance figure of slag specimen in the time of 1000 ℃) of the temperature of growing up.
Figure 11 is for judging slag specimen (is example with the covering slag) liquid phase and begin to generate and the synoptic diagram of the temperature of growing up (slag specimen be moved the synoptic diagram that liquid phase begins to generate).
Figure 12 is for judging slag specimen (is example with the covering slag) liquid phase and begin to generate and the synoptic diagram (synoptic diagram that liquid phase continues to grow up) of the temperature of growing up.
Figure 13 is for judging slag specimen (is example with the covering slag) liquid phase and begin to generate and the synoptic diagram (liquid phase continues to grow up and the not synoptic diagram of slag appears in the edge) of the temperature of growing up.
Figure 14 is for judging slag specimen (is example with the covering slag) liquid phase and begin to generate and the synoptic diagram of the temperature of growing up (liquid phase continues to grow up and the edge slag synoptic diagram that continues to grow up not).
Figure 15 is for judging slag specimen (is example with the covering slag) liquid phase and begin to generate and the synoptic diagram (liquid phase continues to grow up and the edge forms the not shape appearance figure of slag of ring-type) of the temperature of growing up.
Figure 16 melts the process synoptic diagram (ring-type not slag continues to become synoptic diagram big and that begin to melt) that forms liquidus temperature fully for judging slag specimen (is example with the covering slag)
Figure 17 melt the process synoptic diagram that forms liquidus temperature (ring-type not slag constantly melts and isolates the shape appearance figure that graininess or the little slag of reunion shape are considered to be worth doing) fully for judging slag specimen (is example with the covering slag).
Figure 18 judges that slag specimen (is example with the covering slag) melts the process synoptic diagram (ring-type not slag is also constantly fused into the synoptic diagram of liquid phase rapid the decomposition) that forms liquidus temperature fully.
Figure 19 melts the process synoptic diagram (a large amount of not slags have been fused into the synoptic diagram of liquid phase) that forms liquidus temperature fully for judging slag specimen (is example with the covering slag).
Figure 20 melts the process synoptic diagram (liquid phase continues to grow up and the not molten shape appearance figure of part slag specimen is only arranged) that forms liquidus temperature fully for judging slag specimen (is example with the covering slag).
Figure 21 melts the process synoptic diagram (slag specimen melts the synoptic diagram that forms liquid phase fully) that forms liquidus temperature fully for judging slag specimen (is example with the covering slag).
Figure 22 is a high-temperature laser Laser Scanning Confocal Microscope apparatus synoptic diagram.
Embodiment
Below in conjunction with instance; Select two kinds of different slag specimen types of blast furnace slag and covering slag; Observe through two kinds of slag specimen fusion processes being carried out high-temperature metallography; Specify slag specimen in high temperature changes,, and fusion process liquid phase forming core, fusion variation behavior such as grow up carried out brief analysis how from the solid-state whole process that transforms to liquid state.
The accurate mensuration of observation of instance 1 blast furnace slag melting behavior and fusing point
The present invention is applied in observation of blast furnace slag melting behavior and fusing point test, and concrete steps are following:
1. slag specimen preparation.After blast furnace slag calcination to glassy state slag and shrend, grind to form 100 purpose ground-slags.
2. slag specimen moulding.By dextrin and with anhydrous filter paper powder appearance is pushed and to be fixed on the platinum sheet, make the slag specimen moulding.
3. high-temperature laser is adorned appearance.The platinum sheet that the moulding slag specimen is housed is placed Al
2O
3After the crucible bottom, put into the high-temperature metallography heating furnace of high-temperature laser Laser Scanning Confocal Microscope.
4. experimental arrangement setting.Intensification experimental arrangement to blast furnace slag is provided with (see figure 2), vacuumizes the back at Ar
2The experiment of lowering the temperature under the atmosphere protection.
5. fusion process is observed.Through computing machine fusion process is carried out Real Time Observation, and focus on adjustment at any time.
6. picture collection and interpretation of result.After experiment finishes, the blast furnace slag fusion process is carried out image interception, and brief analysis is carried out in fusion process liquid phase forming core, fusion variation behavior such as grow up.Wherein, experiment mainly contains elements such as O, Al, Si, Ca, Ti with blast furnace slag, and Fig. 4～Fig. 9 is the melting behavior synoptic diagram of blast furnace slag in whole temperature-rise period.Interpretation is following:
Fig. 4～Fig. 5 begins to generate the synoptic diagram of temperature for judging slag specimen (is example with the blast furnace slag) liquid phase.In temperature-rise period, the blast furnace slag specimen is not almost having obvious variation below 1000 ℃, when rising to more than 1000 ℃; The surface is changed canescence into by black, and when rising to 1200 ℃, the surface brightens gradually; Vacuole successively appears in the different parts on slag specimen surface, shows that liquid phase begins to generate, and sees Fig. 4.When rising to 1220 ℃, liquid phase increases, and the position that has begins to take place group and gathers the collection phenomenon, sees Fig. 5.
Fig. 6～Fig. 7 is a slag specimen (is example with the blast furnace slag) at temperature-rise period liquid phase forming core, melting behavior synoptic diagram such as grow up.In 1220 ℃ of-1230 ℃ of scopes, sample takes place significantly to shrink, and the position that has begins sharply to move, and liquid phase begins continuous forming core and grows up, and sees Fig. 6.In 1230 ℃ of-1250 ℃ of scopes, the slag specimen surface is convergence type always moves, but mobile comparatively slow, liquid phase continues to grow up, and sees Fig. 7.
Fig. 8～Fig. 9 melts the synoptic diagram that forms liquidus temperature fully for judging slag specimen (is example with the blast furnace slag).Along with temperature continues to raise, slag specimen progressively pools together, and almost completely melts about 1365 ℃ to be liquid state, and final the contraction is spherical.See Fig. 8.Along with the continuation rising of temperature, contraction is spherical liquid phase and begins outwards to spread growth again, no longer changes until 1500 ℃, is a sphere that area is bigger, sees Fig. 9.
By on can know that blast furnace slag can judge that accurately the initial formation temperature of liquid phase is 1200 ℃ through the high-temperature laser Laser Scanning Confocal Microscope at temperature-rise period, and fully fusing to form liquidus temperature be 1365 ℃, thereby realize the fusing point of slag specimen material is accurately measured.
The accurate mensuration of observation of instance 2 covering slag melting behaviors and fusing point
The present invention is applied in observation of covering slag melting behavior and fusing point test, and concrete steps are following:
1. slag specimen preparation.After covering slag calcination to glassy state slag and shrend, grind to form 150 purpose ground-slags.
2. slag specimen moulding.By dextrin and with anhydrous filter paper powder appearance is pushed and to be fixed on the platinum sheet, make the slag specimen moulding.
3. high-temperature laser is adorned appearance.The platinum sheet that the moulding slag specimen is housed is placed Al
2O
3After the crucible bottom, put into the high-temperature metallography heating furnace of high-temperature laser Laser Scanning Confocal Microscope.
4. experimental arrangement setting.Intensification experimental arrangement to covering slag is provided with (see figure 3), vacuumizes the back at Ar
2The experiment of lowering the temperature under the atmosphere protection.
5. fusion process is observed.Through computing machine fusion process is carried out Real Time Observation, and focus on adjustment at any time.
6. picture collection and interpretation of result.After experiment finishes, the covering slag fusion process is carried out image interception, and brief analysis is carried out in fusion process liquid phase forming core, fusion variation behavior such as grow up.Wherein, experiment mainly contains elements such as O, Ba, Al, Si, Ca, Na, Mg with floride-free covering slag, and Figure 10～Figure 21 is the melting behavior synoptic diagram of covering slag in whole temperature-rise period.Interpretation is following:
Figure 10 is the apparent shape appearance figure of covering slag in the time of 1000 ℃, and the edge of slag specimen appears irregularly shaped, and slag specimen is black still, show slag under 1000 ℃ fusing characterize; Along with temperature raises, the slag specimen color is shoaled by black gradually, when rising to 1412 ℃; Slag specimen becomes grey black; And take place from inside to outside suddenly slowly to move, the edge is by uneven also become gradually level and smooth (seeing Figure 11), in the time of 1425 ℃; The slag specimen edge becomes slick and sly (seeing Figure 12) fully, can judge that thus the temperature that liquid phase begins to generate is 1412 ℃.
Afterwards; Along with temperature constantly raises, slag specimen continues fusing and outwards spreads to grow up, but the not slag that short texture and color are shallower than heart portion slag specimen appears in the edge; These are slag when platinum sheet edge spreads in the same way with slag specimen main body one not; Sprawl more and more widelyer, more and more thinner, its color also becomes canescence by grey black, sees Figure 13-15.When temperature rose to 1500 ℃, the slag part had not formed a tangible annulus, sees Figure 15.
In the process of 1500 ℃ of insulation 20min, the ring-type not width of slag continue to become big, up to the edge junction of platinum sheet, and structure becomes more loose, sees Figure 16.Along with holding time prolonging; Become the most loose with the not slag of slag intersection, and constantly have the little slag bits of graininess or reunion shape to break away from not slag of ring-type, ring-type is destroyed gradually; The little slag bits that of dissociating get into liquid interface and constantly are melted, and see Figure 17.When insulation 400s, ring-type not slag is decomposed rapidly and is constantly fused into liquid phase, and the liquid state that the interface place is light becomes wideer, and slag is not fused into liquid phase in a large number, sees Figure 18.When insulation 700s, liquid phase constantly spreads and grows up, and only has the part slag specimen near platinum sheet edge to melt, and the slag specimen fusing characterizes sees Figure 19.During insulation 800s, liquid phase is engulfed solid slag fully and is characterized obviously, shows as liquid phase and moves rapidly, and expansion is very fast, and it is not molten only to deposit several particles, sees Figure 20.During insulation 1000s, slag specimen is fine melt (seeing Figure 21), because quantity of sampling quantity is on the high side, during the slag specimen fine melt, fails to appear obviously contraction-like.
Visible by above two instances, in temperature-rise period, different slags all can judge that accurately slag charge changes into the initial temperature of fusion of liquid phase and the temperature of fusion that is completed into liquid phase from solid phase, accurately measures the slag specimen fusing point through the high-temperature laser Laser Scanning Confocal Microscope.
In addition, can Real Time Observation arrive through the high-temperature laser Laser Scanning Confocal Microscope, different slags are in the high temperature melting process, and hot properties that is shown and liquid phase melting behavior are not quite similar.And the different characteristic that different slag specimens are appeared in the high-temperature fusion process and some complicated variations can be used as the important means of estimating different slag specimen hot properties.
Claims (1)
1. the method for slag class material melts behavior and fusing point test is characterized in that processing step is following:
(1) slag specimen preparation: slag charge is placed platinum/graphite crucible, in opened type agitating heating stove, carry out 1400～1550 ℃ of calcinations of high temperature, behind calcination to the glassy state slag, shrend; Again with cooled slag specimen through the disintegrating apparatus fragmentation after, with agate mortar fully grind, mixing processes 50～200 purpose ground-slags;
(2) slag specimen moulding: by dextrin that powder appearance is bonding, and with anhydrous filter paper the ground-slag applying light is fixed on 3mm * 3mm platinum sheet, make the slag specimen moulding;
(3) high-temperature laser dress appearance: the platinum sheet that the moulding slag specimen will be housed places the Al of Φ 8mm * 4mm
2O
3The bottom of crucible is again with Al
2O
3Crucible is put into 100～1700 ℃ of metallographic heating furnaces of high temperature of laser confocal microscope;
(4) experiment parameter setting: will place the slag specimen of metallographic heating furnace to carry out vacuum pumping earlier, setting heating rate according to different slag class materials again is 60～600 ℃/s, and temperature is 1300～1600 ℃, then at Ar
2Experiment heats up under the atmosphere protection;
(5) fusion process is observed: can carry out Real Time Observation to fusion process through computing machine, and synchronous acquisition needs in the observation process to focus on adjustment at any time according to the sharpness of image to the dynamic menu of whole fusion process; Wherein, the initial temperature of fusion of slag specimen raises with temperature to observe solid-state slag specimen that to begin to occur vacuole be sign; Slag specimen is completed into the temperature of fusion of liquid phase and sharply shrinks to observe solid-liquid coexistence slag specimen surface, has only liquid slag to exist for sign until being converted into fully;
(6) data and Flame Image Process: after experiment finishes, preserve experimental data and results for video, the initial temperature of fusion of intercepting and be completed into the corresponding typical picture of the temperature of fusion of liquid phase and liquid phase forming core, the fusion of growing up change the behavior video and analyze.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110402527 CN102495096B (en) | 2011-12-06 | 2011-12-06 | Method for determining melting behavior and melting point of slag-like material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110402527 CN102495096B (en) | 2011-12-06 | 2011-12-06 | Method for determining melting behavior and melting point of slag-like material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
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| CN103235000A (en) * | 2013-04-18 | 2013-08-07 | 首钢总公司 | Experimental method for determining fusion characteristics of coal ash for spraying |
| CN103994997A (en) * | 2014-05-15 | 2014-08-20 | 首钢总公司 | Method for detecting soft heating property of iron-containing raw material for blast furnace |
| CN104407007A (en) * | 2014-12-16 | 2015-03-11 | 中南大学 | Method for determining melting temperature interval and melting behavior of metallurgical slag |
| CN104597071A (en) * | 2015-02-10 | 2015-05-06 | 攀枝花学院 | Measurement method for relative softening temperature of carbon-sulphur crucible |
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| CN103994997A (en) * | 2014-05-15 | 2014-08-20 | 首钢总公司 | Method for detecting soft heating property of iron-containing raw material for blast furnace |
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| CN113834845A (en) * | 2020-06-24 | 2021-12-24 | 中国科学院金属研究所 | Method for measuring melting temperature range of titanium and titanium alloy by differential thermal analysis method |
| CN112147175A (en) * | 2020-08-28 | 2020-12-29 | 西安建筑科技大学 | Method for measuring high-temperature physicochemical property of lead slag |
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| CN115452655A (en) * | 2022-09-06 | 2022-12-09 | 燕山大学 | Application of reduced melting entropy in evaluating melting point viscosity of molecular system and method |
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