CN101407866A - Fe-Ti-N grain refiner of steel and preparation thereof - Google Patents
Fe-Ti-N grain refiner of steel and preparation thereof Download PDFInfo
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- CN101407866A CN101407866A CNA2008102030237A CN200810203023A CN101407866A CN 101407866 A CN101407866 A CN 101407866A CN A2008102030237 A CNA2008102030237 A CN A2008102030237A CN 200810203023 A CN200810203023 A CN 200810203023A CN 101407866 A CN101407866 A CN 101407866A
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Abstract
The invention relates to a Fe-Ti-N grain refiner of steel in the technical field of metal materials and a preparation method thereof. The components and the weight percentage ratio of the grain refiner are as follows: 35 to 99.4 percent of Fe, 0.5 to 50 percent of Ti and 0.1 to 15 percent of N. The grain refiner has dispersively distributed TiN particles. The method is as follows: 40 to 99.5 percent of pure iron and 0.5 to 60 percent of Ti are arranged into the crucible of a vacuum middle-frequency induction furnace for heating and melting; the temperature of a fused mass is maintained between 1550 and 1650 DEG C; nitrogen is introduced into the vacuum middle-frequency induction furnace and the sub-pressure of the nitrogen in the furnace is maintained between 0.01 and 0.1MPa; an aeration pipe is inserted into the fused mass of alloy for blowing nitrogen; and after a preset time is reached, the aeration pipe is taken out and the power is off for casting. After the fused mass of steel is added with less Fe-Ti-N grain refiner of steel obtained by the method, the isometric crystal grain size of cast structure is greatly reduced; the proportion of isometric area is improved to more than 60 percent; and the refining effect of the grain refiner is remarkable.
Description
Technical field
The present invention relates to grain-refining agent of a kind of metallic substance technical field and preparation method thereof, specifically is Fe-Ti-N grain-refining agent of a kind of steel and preparation method thereof.
Background technology
Ultra-fine crystallization theory and technology are the cores of development iron structure material of new generation, solidify refinement and then be key basic technology wherein.In the casting process, if only from exterior cooling, the speed of cooling of generous inside steel billet is slow, and the forming core core is few, with mainly growing in the mode of column crystal, causes defectives such as crystal grain is thick, center segregation, is easy to generate limit portion crackle when subsequent hot rolled.The key that addresses this problem is to enlarge strand equiax crystal district ratio, crystal grain thinning.Controlling metal solidification texture by the interpolation nucleating agent is the crystal fining method of using always, and purpose is the formation that reduces dendrite interval, promotion equiax crystal, the growth that suppresses column crystal.The forming core core mainly contains two kinds of sources: external forming core particle and Nei Sheng forming core particle.Wherein, mainly be to point in the melt to add grain-refining agent by increasing the method that external forming core particle reaches the refinement purpose.
Find through literature search prior art, " adding the super particulate research of titanium nitride in the high temperature pure iron melt " (steel vanadium titanium of delivering such as holds in kingdom, 2006,27 (2): 21~25), this technology adopts and add TiN particulate method refined cast structure in the pure iron melt.Because the TiN particle is more tiny, be difficult to it be added in the melt with the method for winding-up, hello silk, and poly-partially easily.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, Fe-Ti-N grain-refining agent of a kind of steel and preparation method thereof is provided, method with logical nitrogen in the Fe-Ti alloy melt prepares the Fe-Ti-N grain-refining agent, the TiN particle that utilizes generated in-situ a large amount of small and disperseds distributions in the matrix is finally realized the refinement of steel billet as-cast structure crystal grain and the technology that improves its proportion of equiaxed grain as heterogeneous forming core core.
The present invention is achieved by the following technical solutions:
The Fe-Ti-N grain-refining agent of steel involved in the present invention, component that comprises and weight percent thereof are: Fe 35-99.4%, Ti 0.5-50%, N 0.1-15% has the TiN particle that disperse distributes in this grain-refining agent.
The TiN pellet density reaches 10000/mm at least in the described grain-refining agent
3
The TiN particle size concentrates on (0.5-3 μ m) in the described grain-refining agent.
The preparation method of the Fe-Ti-N grain-refining agent of steel involved in the present invention comprises the steps:
The first step is that the pure iron of 40-99.5% and the Ti of 0.5-60% put into the fusing of vacuum medium frequency induction furnace crucible internal heating with weight ratio, and melt temperature remains on 1550-1650 ℃.
In second step, logical nitrogen in vacuum medium frequency induction furnace makes the interior nitrogen partial pressure of stove remain on 0.01-0.1MPa.
The 3rd step, ventpipe is inserted the alloy melt nitrogen blowing, nitrogen flow is constant in 100ml/min to 1000ml/min.
The 4th step, after air blowing reaches the scheduled time, extract ventpipe out, the outage casting promptly obtains the Fe-Ti-N grain-refining agent of steel.
In the first step, adopt thermocouple temperature measuring apparatus on-line measurement temperature, make melt temperature remain on 1550-1650 ℃.
In the 4th step, the scheduled time is meant 10s-3h.
The present invention is by the original position generating principle, the technology for preparing the grain-refining agent of steel by the method for logical nitrogen in the Fe-Ti alloy melt, go on foot the N that in stove, leads to nitrogen and the introducing of melt generation chemical reaction by second step and the 3rd, prepare the gained grain-refining agent and adopt heart yearn or be broken into the adding before the molten steel casting of granular mode, and the TiN particle dispersion as heterogeneous forming core core is distributed in the melt after adding.After adding the preparation-obtained Fe-Ti-N grain-refining agent of a small amount of the present invention of employing in the melt of steel, as-cast structure equiax crystal grain-size reduces greatly, and equiax crystal district ratio is brought up to more than 60%, and the thinning effect of grain-refining agent is obvious.
Description of drawings
The device synoptic diagram that Fig. 1 adopts for the embodiment of the invention.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
As shown in Figure 1, the setting drawing that present embodiment adopts is among the figure: the 1-threeway; 2, the 3-ball valve; 4-nitrogen flow meter; 5, the 6-nitrogengas cylinder; The 7-ruhmkorff coil; The 8-temperature measurer; The 9-crucible; The 10-thermopair; 11-nitrogen; The 12-ventpipe; The 13-melt.The pure iron of 50-99.5% and the Ti of 0.5-50% are put into the fusing of vacuum medium frequency induction furnace crucible 9 internal heating, adopt thermocouple temperature measuring apparatus 7,8 on-line measurement temperature, make melt 13 temperature remain on 1550-1650 ℃.Open ball valve 3 by nitrogengas cylinder 6 logical nitrogen 11 in stove, make the interior nitrogen partial pressure of stove remain on 0.01-0.1MPa.Open ball valve 2 after closing ball valve 3, regulate nitrogen flow meter 4 and make the air-flow of nitrogengas cylinder 5 outputs constant at (100-1000ml/min).Ventpipe 12 is inserted in the Fe-Ti alloy melt 13.After ventilation reaches the scheduled time (10s-3h), extract ventpipe 12 out, the outage casting promptly obtains the grain-refining agent of steel.
Embodiment:
Heat fused Fe-Ti alloy under vacuum condition, (here the mass percent pointer of ferrotitanium is to the ratio of two kinds of elements of ferrotitanium to contain the pure iron of 40-99.5% and the Ti of 0.5-60% in the alloy, wherein do not comprise N), when melt temperature constant in (1550-1650 ℃) scope the time in burner hearth logical nitrogen.When nitrogen partial pressure in the stove reaches (0.01-0.1Mpa), ventpipe is inserted the alloy melt nitrogen blowing, nitrogen flow is constant in 100ml/min to 1000ml/min.Gassing time is controlled at 10s to 3h.The TiN particle size mainly concentrates on (0.5-3 μ m) in the preparation gained grain-refining agent.
Among the embodiment 1 in the preparation gained grain-refining agent TiN density be 10
4Individual/mm
3
Among the embodiment 2 in the preparation gained grain-refining agent TiN pellet density be 10
7Individual/mm
3
Among the embodiment 3 in the preparation gained grain-refining agent TiN density be 10
8Individual/mm
3
Embodiment | Fe mass percent % | Ti mass percent % | N mass percent % | Temperature of reaction ℃ | Nitrogen flow ml/min | Blow the scheduled time | Nitrogen partial pressure MPa in the |
1 | 99.4 | 0.5 | 0.1 | 1650 | 1000 | 3h | 0.1 |
2 | 67.5 | 25 | 7.5 | 1600 | 500 | 1.5h | 0.05 |
3 | 35 | 50 | 15 | 1550 | 100 | 10s | 0.01 |
Fe only plays carrier function in fining agent, do not play refining effect, and the key of fining agent is to play the TiN particulate density of heterogeneous forming core core.
The foregoing description is to adopt the method original position that feeds nitrogen in the Fe-Ti alloy melt to generate to have the TiN particulate Fe-Ti-N grain-refining agent that a large amount of disperses distribute; In steel melt, add the Fe-Ti-N grain-refining agent, utilize TiN particle in the matrix as the heterogeneous forming core core of steel, thereby the crystal grain of refinement steel, and the ratio of steel billet as-cast structure equiax crystal is brought up to more than 60%, the technology of preparation master alloy is simple, easy to use, with low cost, pollution-free.
Claims (6)
1, a kind of Fe-Ti-N grain-refining agent of steel is characterized in that, component that comprises and weight percent thereof are: Fe 35-99.4%, and Ti 0.5-50%, N 0.1-15% has the TiN particle that disperse distributes in this grain-refining agent.
2, the Fe-Ti-N grain-refining agent of steel according to claim 1 is characterized in that, the TiN pellet density reaches 10000/mm at least in the described grain-refining agent
3
3, the Fe-Ti-N grain-refining agent of steel according to claim 1 is characterized in that, the TiN particle size is between 0.5 μ m-3 μ m in the described grain-refining agent.
4, a kind of preparation method of Fe-Ti-N grain-refining agent of steel as claimed in claim 1 is characterized in that, comprises the steps:
The first step is that the pure iron of 40-99.5% and the Ti of 0.5-60% put into the fusing of vacuum medium frequency induction furnace crucible internal heating with weight ratio, and melt temperature remains on 1550-1650 ℃;
In second step, logical nitrogen in vacuum medium frequency induction furnace makes the interior nitrogen partial pressure of stove remain on 0.01-0.1Mpa;
The 3rd step, ventpipe is inserted the alloy melt nitrogen blowing, nitrogen flow is constant in 100ml/min to 1000ml/min;
The 4th step, after air blowing reaches the scheduled time, extract ventpipe out, the outage casting promptly obtains the grain-refining agent of steel.
5, the preparation method of the Fe-Ti-N grain-refining agent of steel according to claim 4 is characterized in that, in the first step, adopts thermocouple temperature measuring apparatus on-line measurement temperature, makes melt temperature remain on 1550-1650 ℃.
6, the preparation method of the Fe-Ti-N grain-refining agent of steel according to claim 4 is characterized in that, in the 4th step, the scheduled time is meant 10s-3h.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108642241A (en) * | 2018-06-05 | 2018-10-12 | 东北大学 | A kind of ferritic stainless steel grain refiner, preparation method and application |
CN113604726A (en) * | 2021-07-29 | 2021-11-05 | 三鑫重工机械有限公司 | Preparation method of in-situ regeneration titanium nitride steel-based roller |
-
2008
- 2008-11-20 CN CN2008102030237A patent/CN101407866B/en not_active Expired - Fee Related
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108642241A (en) * | 2018-06-05 | 2018-10-12 | 东北大学 | A kind of ferritic stainless steel grain refiner, preparation method and application |
CN113604726A (en) * | 2021-07-29 | 2021-11-05 | 三鑫重工机械有限公司 | Preparation method of in-situ regeneration titanium nitride steel-based roller |
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