CN104406893B - Method for measuring dissolution speed of solid inclusion in slag - Google Patents
Method for measuring dissolution speed of solid inclusion in slag Download PDFInfo
- Publication number
- CN104406893B CN104406893B CN201410624238.1A CN201410624238A CN104406893B CN 104406893 B CN104406893 B CN 104406893B CN 201410624238 A CN201410624238 A CN 201410624238A CN 104406893 B CN104406893 B CN 104406893B
- Authority
- CN
- China
- Prior art keywords
- slag
- dissolution
- inclusion
- inclusion particle
- rate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Treatment Of Steel In Its Molten State (AREA)
Abstract
The invention discloses a method for measuring the dissolution speed of solid of solid inclusion in slag, and belongs to the technical field of metallurgy. The method comprises the following steps: (1) in an inert gas atmosphere, heating slag to a temperature 150 to 200 DEG C higher than the melting point of the slag to form molten slag, and then maintaining the temperature; (2) adding inclusion particles into the molten slag, and evenly stirring; (3) sampling the molten slag by a sampling device, and cooling the sample in a cooling table until the sample is completely cured to form a metallographic sample; (4) observing the metallographic sample by a metallographic microscope and a scanning electron microscope, analyzing and calculating the equivalent diameters, and drawing a curve that represents the relationship between the equivalent diameter and the time; (5) calculating the dissolution speeds of inclusion particles in corresponding slag systems according to the curve and formula. The provided method can visually, precisely, and rapidly measure the dissolution speed of typical inclusions in specific slag system, and thus provides important references for design and optimization of slag systems in the steel making process.
Description
Technical field
The invention belongs to metallurgical technology field, particularly to a kind of mensure side of solid inclusions rate of dissolution in slag
Method.
Background technology
For steel industry, the removal of field trash and its to control be an important content, molten slag is to being mingled with
The absorption of thing and dissolving be inclusion removal a kind of important way.
For rely on the resistance heat of slag system to carry out the electroslag remelting of metal material melting using fluorine-containing slag system, its process
Why there is the ability removing field trash in consutrodes, be also mainly the absorption with fluorine-containing slag system to field trash for the electroslag metallurgy
And dissolution.During electroslag metallurgy, after consutrodes melt in high-temperature liquid state slag bath, can constantly form little molten drop and drip
Fall, can be fully contacted with melt cinder during little molten drop formation and drippage, the removal of steel inclusion occurs mainly in this stage,
And this process duration is very short, how fast and effeciently to remove steel inclusion is the important of impact end product quality
Process.However, different slag systems is different to the absorption solvability of steel inclusion, for many years, numerous metallargists, pass through
After different slag system remeltings, the method such as the analysis content of nonmetallic inclusionsin steel, type, size is optimizing setting of slag system
Meter, however, this method is affected and restriction by many factors；First, under industrial process conditions plus during slag, have very
Many granulated slags fly away and affect slag charge composition and affect final analysis and judgement；Secondly, the quantitation of nonmetallic inclusionsin steel is non-
Often difficult.Many researchers carry out quantitation by the method for quantitative metallography to steel inclusion, but are difficult to prepare non-convention
The metallographic specimen thought, in research process, prepared metallographic specimen suffers from extraneous factor interference and affects result accuracy；Again
Have, final electroslag steel inclusion is most to be secondary generation, and this is mainly affected by oxygen content in steel, and oxygen content in steel with outer
It is relevant that boundary's air passes oxygen by molten slag in steel.
Common method for making steel to Control and Inclusion Removal aspect, also mainly pass through to optimize composition range in phasor for the slag system,
The method of the common physical and chemical performance such as working the slag basicity, fusion temperature, viscosity, and carry out comprehensive tune with reference to some other operational means
Section slag system is to the removal of steel inclusion and control ability.But no matter which kind of method for making steel, the quick absorption to field trash for the slag system
It is the important prerequisite of Control and Inclusion Removal with dissolving.
In sum, at present, the method for designing of traditional slag system carries out slag system and controls the research of steel inclusion ability is to have
Circumscribed, especially at present, high end materials (special steel or special alloy) are all to be prepared under protective atmosphere, and this is just
Eliminate the interference of ambient atmosphere environment；Under these conditions, slag system itself, to the absorption of steel inclusion and dissolving, just determines
The content of final steel inclusion.Therefore, set up a kind of method, study the rate of dissolution to steel inclusion for the slag system, in steel
The control of field trash has great importance.
Content of the invention
It is an object of the invention to provide a kind of assay method of solid inclusions rate of dissolution in slag, by slag
Middle addition inclusion particle, cools down after different periods sampling and makes metallographic specimen, then be observed and analyze, obtain granularity
Or rate of dissolution changes over curve, rapidly, truly measure solid inclusions rate of dissolution in slag to reach
Purpose, the design for reasonable slag system provides important reference frame.
The solid inclusions of present invention assay method of rate of dissolution in slag sequentially includes the following steps:
1st, under inert atmosphere conditions, temperature slag charge being heated above 150 ~ 200 DEG C of its fusing point forms slag, insulation
10 ~ 15min makes slag composition full and uniformization；
2nd, inclusion particle is added in slag by funnel, stirring 3 ~ 5s makes inclusion particle uniformly divide in slag
Cloth；
3rd, in different time sections, separately sampled in slag by sampler；The slag specimen of taking-up is placed in cold on cooling stage
But to solidifying, then it is respectively prepared metallographic specimen；
4th, each metallographic specimen made is carried out observing under metallurgical microscope and scanning electron microscope, the shape of analysis field trash
Be converted to equivalent diameter with size and by its size, draw different time points materialsed middle inclusion particle equivalent diameter with
The change curve of time；
5th, rate of dissolution under corresponding slag system ingredient for the inclusion particle is calculated according to above-mentioned change curve and formula, described
Formula be:
Wherein,For the rate of dissolution of inclusion particle, unit is μm s-1, r is the radius of alumina particle, and unit is μ
m；T is the time, and unit is s.
In said method, inclusion particle addition presses the weight of field trash and slag charge than for 1:(10 ~ 15), described folder
The particle size range of inclusion particles is at 250 ± 25 μm.
In said method, the time interval of step 3 sampling is 30 ~ 300s, and the time interval measuring sampling every time is equal.
In said method, when measure inclusion particle in electroslag metallurgy with the rate of dissolution in fluorine-containing slag system when, adopt two
Root electrode inserts energising the thermodynamic condition with slag composition power circuit simulation electroslag metallurgy process in slag.
The inclusion particle that said method is selected is alumina particle.
Above-mentioned cooling stage is from flat board, material selection pure iron or the fine copper with barrel-shaped groove.
The device that said method step 1 ~ 3 adopt includes electric furnace and crucible, and crucible is located in the boiler tube of electric furnace,
The refractory brick of boiler tube puts and is provided with gas tube and charge door, and temperature thermocouple is in the lower flange insertion boiler tube of electric furnace.
In above-mentioned device, in the refractory brick set insertion crucible of boiler tube, two electrodes pass through wire and electricity to two electrodes
Source connects.
The using method of said apparatus is: noble gases is filled with into boiler tube by gas tube and keeps circulating, then by earthenware
Slag is made in slag charge heating in crucible；Place funnel in charge door, then inclusion particle is added by funnel, to ensure to be mingled with
Composition granule can all add in slag；When needing sampling, funnel shifter is removed, using the sampler of molybdenum filament and crucible composition
Take slag specimen from charge door insertion slag bath, slag specimen is placed on the cooling groove on cooling stage Nei after taking out.
When measure field trash in electroslag metallurgy with the rate of dissolution in fluorine-containing slag system when, by power supply to the two poles of the earth energising, and
Constitute power circuit with slag, simulate electroslag metallurgy process.
It is molten in specific slag system that the method for the present invention can intuitively, exactly, rapidly determine typical field trash
Solution speed, thus the design for steelmaking process slag system and optimization provide important reference frame.
Brief description
Fig. 1 is the apparatus structure schematic diagram in the embodiment of the present invention；In figure, 1, power supply, 2, wire, 3, funnel, 4, inflation
Pipe, 5, refractory brick set, 6, bell, 7, body of heater, 8, boiler tube, 9, crucible, 10, inclusion particle, 11, slag, 12, heater, 13,
Refractory material, 14, temperature thermocouple, 15, lower flange, 16, gas cylinder；
Fig. 2 is the sampler structure schematic diagram in the embodiment of the present invention；In figure, 17, molybdenum filament, 18, sampling crucible；
Fig. 3 is the side view of Fig. 2；
Fig. 4 is the top view of Fig. 2；
Fig. 5 is the cooling stage structural representation in the embodiment of the present invention；
Fig. 6 is that figure is cutd open in the side-looking of the cooling stage in the embodiment of the present invention；
Fig. 7 is the equivalent diameter versus time curve figure of the inclusion particle of the embodiment of the present invention 1；
Fig. 8 is the equivalent diameter versus time curve figure of the inclusion particle of the embodiment of the present invention 2；
Fig. 9 is the equivalent diameter versus time curve figure of the inclusion particle of the embodiment of the present invention 3.
Specific embodiment
The metallographic specimen preparation accepted standard adopting in the embodiment of the present invention is gb/t 13298-91 or astm e3-
01.
The method analyzed the shape and size of field trash in the embodiment of the present invention and its size is converted to equivalent diameter is:
Calculate the area of field trash by image-pro plus 6.0 software first, then according to method calculating of equivalent diameter etc.
Effect diameter.
The metallurgical microscope model axio imager m2m type adopting in the embodiment of the present invention；
Scanning electron microscope model ssx-550 type is adopted in the embodiment of the present invention；
The noble gases adopting in the embodiment of the present invention are argon.
The inclusion particle adopting in the embodiment of the present invention is alumina particle, and particle size range is at 250 ± 25 μm.
Embodiment 1
The apparatus structure that molten slag dissolving adopts is as shown in figure 1, include electric furnace and crucible 9；Electric furnace includes
Refractory brick set 5, bell 6, body of heater 7, boiler tube 8, heater 12, refractory material 13, lower flange 15；Crucible 9 is located in boiler tube 8, resistance to
Firebrick set 5 is provided with gas tube 4 and charge door, and temperature thermocouple 14 inserts in boiler tube 8 from lower flange 15；
Funnel 3 is placed with charge door；Gas tube 4 is connected with gas cylinder 16；
In refractory brick set 5 insertion crucible 9, two electrodes are connected with power supply 1 two electrodes by wire 2；
Cooling stage structure is as it can be seen in figures 5 and 6, carry flat board, material selection pure iron or the fine copper of barrel-shaped groove；
Sampler structure as shown in Fig. 2,3 and 4, including the molybdenum filament 17 being fixed together and sampling crucible 18；
Method sequentially includes the following steps:
1st, under inert atmosphere conditions, temperature slag charge being heated above 150 ~ 200 DEG C of its fusing point forms slag, insulation
10min makes slag composition full and uniformization；
2nd, inclusion particle is added in slag by funnel, stirring 3 ~ 5s makes inclusion particle uniformly divide in slag
Cloth；Inclusion particle addition presses the weight of field trash and slag charge than for 1:10；
3rd, in different time sections, separately sampled in slag by sampler；The slag specimen of taking-up is placed in cold on cooling stage
But to solidifying, then it is respectively prepared metallographic specimen；The time interval of sampling is 300s, measures the time interval phase of sampling every time
Deng；
4th, each metallographic specimen made is carried out observing under metallurgical microscope and scanning electron microscope, the shape of analysis field trash
Be converted to equivalent diameter with size and by its size, draw different time points materialsed middle inclusion particle equivalent diameter with
The change curve of time；
5th, rate of dissolution under corresponding slag system ingredient for the inclusion particle is calculated according to above-mentioned change curve and formula, described
Formula be:
Wherein,For the rate of dissolution of inclusion particle, unit is μm s-1, r is the radius of alumina particle, and unit is μ
m；T is the time, and unit is s；
Selected slag system is Tundish Slag, and composition by weight percent is 32.5%cao-35%al2o3-32.5%sio2, try twice
The temperature testing molten slag in temperature is respectively 1773k and 1823k, and every sub-sampling takes two；
The equivalent diameter versus time curve figure of the inclusion particle that step 4 obtains is as shown in Figure 7；
As seen from the figure, the growth almost over time of the size of alumina particle and linearly reduce and with temperature
Increase its rate of dissolution to be consequently increased, the 2.1 when rate of dissolution in 1823k is approximately 1773k times；
For Spherical Inhomogeneity composition granule, its size over time can be given below:
Wherein, dr/dt is the rate of dissolution of field trash, μm/s；It is the mass tranfer coefficient in slag, μm/s；c i 、c b Respectively
It is the al in slag/field trash interface and slag2o3Concentration, mol/cm3；mFor al2o3The molal weight of granule, g/mol；
For the density of alumina particle, g/cm3；
Under specific slag ingredient, specific temperature conditions, in field trash course of dissolution、c i Andc b Vary less, therefore press from both sides
The rate of dissolution of debris increases over time and will not change very greatly, that is, present inclusion particle size and increase with smelting time
Plus and the characteristic of linear reduction；
Based on this, equation below can be obtained:
Wherein,For the original radius of inclusion particle,rBy middle inclusion particle radius of being materialsed；
However, for the slag system of special component, with the increase of temperature, the viscosity of slag reduces, mobility strengthens, its
al2o3Mass tranfer coefficient in slag increases so leading to the rate of dissolution of field trash to increase sharply；
Under the conditions of calculating 1773k and 1823kIt is respectively 0.0733 μm of s-1With 0.1535 μm of s-1.
Embodiment 2
Using device with embodiment 1；Difference is: cooling stage material selection pure iron or fine copper；
With embodiment 1, difference is method:
Slag is incubated 15min；
Inclusion particle addition presses the weight of field trash and slag charge than for 1:15；
The time interval of sampling is 50s；
Selected slag system is two kinds of typical ladle slag, and composition by weight percent is respectively 46%cao-46%al2o3-8%sio2With
42%cao-42%al2o3-16%sio2, in test temperature, the temperature of slag is 1773k；
The equivalent diameter versus time curve figure of the inclusion particle obtaining is as shown in Figure 8；
As seen from the figure, with sio in slag2The increase of content, the rate of dissolution of alumina particle decreases, this be due to
With sio in slag2The increase of content, the viscosity of slag raises, mobility weakens, and reduces al2o3Mass tranfer coefficient in slag from
And reduce its rate of dissolution；
Under the conditions of calculating two kinds of typical ladle slag 1773kIt is respectively 0.4625 μm of s-1With 0.3033 μm of s-1.
Embodiment 3
Using device with embodiment 1；
With embodiment 1, difference is method:
Molten slag is incubated 13min；
Inclusion particle addition presses the weight of field trash and slag charge than for 1:12；
The time interval of sampling is 30s；
Selected slag system is ladle slag and electroslag metallurgy slag, and composition by weight percent is respectively 50%cao-50%al2o3With
40%caf2-30%cao-30%al2o3, when measuring rate of dissolution in electroslag metallurgy slag for the inclusion particle, to two electrodes
Energising simultaneously constitutes power circuit, the thermodynamic condition of simulation electroslag metallurgy process with slag；In test temperature, the temperature of slag is
1773k；
The equivalent diameter versus time curve figure of the inclusion particle obtaining is as shown in Figure 9；
As seen from the figure, at the same temperature, due to electroslag metallurgy caf in fluorine-containing slag2Content be higher than ladle slag in
Content, and caf2Can be effectively improved slag viscosity, strengthen slag mobility, thus increasing al2o3Diffusion system in slag
Number, increases its rate of dissolution, therefore, for this angle, al2o3Electroslag metallurgy with the rate of dissolution in fluorine-containing slag system than
Rate of dissolution in ladle slag and tundish refining slag is big；
Under the conditions of calculating ladle slag and electroslag metallurgy slag 1773kIt is respectively 0.5357 μm of s-1With 1.2167 μm of s-1.
Claims (2)
1. a kind of assay method of solid inclusions rate of dissolution in slag is it is characterised in that sequentially include the following steps:
(1) under inert atmosphere conditions, by slag charge be heated above 150 ~ 200 DEG C of its fusing point temperature formed slag, insulation 10 ~
15min makes slag composition full and uniformization；
(2) inclusion particle is added in slag by funnel, stirring 3 ~ 5s makes inclusion particle be uniformly distributed in slag；
Described inclusion particle addition presses the weight of field trash and slag charge than for 1:(10 ~ 15), the grain of described inclusion particle
Degree scope is at 250 ± 25 μm；
(3) in different time sections, separately sampled in slag by sampler；The slag specimen of taking-up is placed on cooling stage and is cooled to
Solidification, is then respectively prepared metallographic specimen；Described cooling stage is from the flat board with barrel-shaped groove, material selection pure iron
Or fine copper；
(4) by each metallographic specimen made carry out under metallurgical microscope and scanning electron microscope observe, analysis field trash shape and
Its size is simultaneously converted to equivalent diameter by size, draw different time points materialsed middle inclusion particle equivalent diameter at any time
Between change curve；
(5) rate of dissolution under corresponding slag system ingredient for the inclusion particle is calculated according to above-mentioned change curve and formula, described
Formula is:
Wherein,For the rate of dissolution of inclusion particle, unit is μm s-1, r be alumina particle radius, unit be μm；T is
Time, unit is s；
When measure inclusion particle in electroslag metallurgy with the rate of dissolution in fluorine-containing slag system when, using in two electrodes insertion slags
Energising simultaneously constitutes, with slag, the thermodynamic condition that power circuit simulates electroslag metallurgy process.
2. a kind of solid inclusions rate of dissolution in slag according to claim 1 assay method it is characterised in that
The device that step (1) ~ (3) adopt includes electric furnace and crucible, and crucible is located in the boiler tube of electric furnace, the refractory brick of boiler tube
Put and be provided with gas tube and charge door, temperature thermocouple is in the lower flange insertion boiler tube being electrolysed hot stove；The using method of device
For: noble gases are filled with into boiler tube by gas tube and keep circulating, then slag is made in the slag charge heating in crucible；Adding
Material mouth places funnel, then passes through funnel addition inclusion particle, to ensure that inclusion particle can all add in slag；When
When needing sampling, funnel shifter is removed, the sampler using molybdenum filament and crucible composition takes slag specimen, slag specimen from charge door insertion slag bath
It is placed on the cooling groove on cooling stage Nei after taking-up.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410624238.1A CN104406893B (en) | 2014-11-10 | 2014-11-10 | Method for measuring dissolution speed of solid inclusion in slag |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410624238.1A CN104406893B (en) | 2014-11-10 | 2014-11-10 | Method for measuring dissolution speed of solid inclusion in slag |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104406893A CN104406893A (en) | 2015-03-11 |
| CN104406893B true CN104406893B (en) | 2017-02-01 |
Family
ID=52644540
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410624238.1A Active CN104406893B (en) | 2014-11-10 | 2014-11-10 | Method for measuring dissolution speed of solid inclusion in slag |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104406893B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105588781B (en) * | 2016-03-09 | 2018-05-04 | 东北大学 | A kind of device and method for measuring field trash rate of dissolution in metallurgy clinker |
| CN109270239A (en) * | 2017-07-13 | 2019-01-25 | 鞍钢股份有限公司 | A kind of slag absorbs the evaluation method of field trash ability |
| CN109114981B (en) * | 2018-07-12 | 2020-01-07 | 东北大学 | Device and method for experimental study of high-temperature reaction of slag metal in metallurgical process |
| CN109298016B (en) * | 2018-08-24 | 2021-04-30 | 上海大学 | Experimental device for simulating iron layer of blast furnace hearth |
| CN110988015A (en) * | 2019-12-30 | 2020-04-10 | 重庆大学 | Hot wire method-based dynamic and interface behavior test method for dissolving solid oxide in molten slag |
| CN111398332A (en) * | 2020-03-23 | 2020-07-10 | 电子科技大学 | System and method for representing dissolution amount and dissolution rate of ceramic in liquid glass at high temperature |
| CN114252440A (en) * | 2021-12-31 | 2022-03-29 | 东北大学 | Contrast detection method for determining content of diboron trioxide in metallurgical slag system |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2010347572B8 (en) * | 2010-03-05 | 2014-12-18 | Loesche Gmbh | Preparation method for stainless steel slags and steelmaking slags for recovering metal |
| CN103468965B (en) * | 2013-09-25 | 2015-04-15 | 安徽工业大学 | Preparation method for electro-slag remelting refining slag efficiently utilizing return slag |
-
2014
- 2014-11-10 CN CN201410624238.1A patent/CN104406893B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104406893A (en) | 2015-03-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104406893B (en) | Method for measuring dissolution speed of solid inclusion in slag | |
| CN105463188B (en) | A kind of method for determining iron ore powder sintering Liquid phase flowability energy | |
| CN104384460B (en) | Standard sample for spectrochemical analysis steel production technology and apparatus for pouring thereof | |
| CN105588781B (en) | A kind of device and method for measuring field trash rate of dissolution in metallurgy clinker | |
| Qi et al. | Investigation on heat transfer performance of fluoride-free and titanium-bearing mold fluxes | |
| WO2014186919A1 (en) | High-hardness aluminum alloy ingot and production method thereof | |
| CN104330411B (en) | Device and method for dynamically observing and simulating behaviors of molten drops in electric slag remelting process | |
| CN105699412A (en) | Testing device and testing method for metal rapid solidification heat flow | |
| Wang et al. | Influence of Al2O3 content on crystallization behaviors of blast furnace slags in directional solidification process | |
| CN107505226A (en) | The distribution of gold and silver in a kind of Fire Assaying enrichment cupel | |
| CN105241915B (en) | A kind of application process of the device of test high-temperature metallurgical slag performance | |
| CN102879130A (en) | Continuous-casting casting powder comprehensive heat transfer heat flow testing method | |
| Ren et al. | Dissolution of SiO2 inclusions in CaO-SiO2-based slags in situ observed using high-temperature confocal scanning laser microscopy | |
| CN206052206U (en) | A kind of sapphire single-crystal furnace | |
| CN103994997B (en) | A kind of method for detecting blast furnace with iron-bearing material reflow conductor roll | |
| CN102890098A (en) | Analytical method for iron ore high-temperature soft melting characteristics | |
| Shevchenko et al. | Experimental liquidus studies of the Pb-Cu-Si-O system in equilibrium with metallic Pb-Cu alloys | |
| CN116121548B (en) | Method, system and equipment for controlling local solidification time of cast ingot in electroslag remelting | |
| Dong et al. | Effective thermal conductivity of slag crust for ESR slag | |
| CN109114981B (en) | Device and method for experimental study of high-temperature reaction of slag metal in metallurgical process | |
| Dong et al. | Temperature distribution of electroslag casting with liquid metal using current conductive ring | |
| CN107576679A (en) | A kind of method for the ESR ingot Local cooling speed for demarcating electroslag remelting production high-speed steel process | |
| CN104032069A (en) | Device for simultaneously sampling and measuring temperature, converter used for steelmaking and method for converter blowing | |
| CN204287055U (en) | The device of a kind of dynamic observation analog electrical slag reflow process molten drop behavior | |
| CN102247902B (en) | Double-crucible experimental apparatus for high-temperature experiment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |