CN104233042A - Smelting method of nanoparticle dispersion strengthened steel - Google Patents
Smelting method of nanoparticle dispersion strengthened steel Download PDFInfo
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- CN104233042A CN104233042A CN201410473694.0A CN201410473694A CN104233042A CN 104233042 A CN104233042 A CN 104233042A CN 201410473694 A CN201410473694 A CN 201410473694A CN 104233042 A CN104233042 A CN 104233042A
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Abstract
The invention provides a smelting method of nanoparticle dispersion strengthened steel. The smelting method comprises the steps as follows: S100, a to-be-smelted material is placed in a smelting container, then the smelting container is placed in a magnetic suspension furnace for smelting treatment to obtain molten steel, the temperature of the magnetic suspension furnace in the smelting treatment is higher than 1500 DEG C, and the smelting time is longer than or equal to 0.5 min, wherein the to-be-smelted material contains large-particle inclusions and titanium; S200, the molten steel is cooled to obtain the nanoparticle dispersion strengthened steel. The nano-scale (10 nm) particle dispersion strengthened super-steel is obtained with the smelting method, a new feasible technology is provided for industrial-scale mass production of ODS (oxide dispersion strengthened) steel, the ODS steel production efficiency can be greatly improved, and the production cost of the ODS steel can be reduced.
Description
Technical field
The present invention relates to field of steel metallurgy, particularly relate to a kind of nano-scale oxide precipitate particle Dispersed precipitate that adopts on the matrix of steel, thus the smelting process of strengthening steel.
Background technology
The type of steel inclusion, form, size and distribution etc. have important impact to the performance of steel, and it mainly exists with nonmetal chemical combination state.Non-metallic inclusion in steel is as the submicroscopic defect of steel inside, when its size is comparatively large or pattern is irregular, easily bring out stress concentration or piling up of dislocations, thus cause steel to produce mechanical heterogeneity when hot-work or cold deformation, easily tired or reduce intensity and toughness.For most steel grade, the performance of the Large Inclusions that size is more than 50 μm on steel just has impact, 1 micron dimension and following little inclusion thereof solidify with the operation of rolling in can be used as the heterogeneous forming core core of sulfide, carbide and nitride, by controlling the size of inclusion, form, quantity, composition and distribution, the performance of steel can be improved.
Aluminium killed steel when continuous casting, dystectic Al
2o
3impact casting on the mouth of a river that inclusion is easily bonded at tundish; Large and concentrated inclusion is very harmful to the performance of steel, and the inclusion of distribute disperse and fine particle, not only can reduce the infringement to Steel Properties, effectively can also improve the performance of steel simultaneously.Such as at room temperature, Al
2o
3when particle is greater than 1 μm, the yield strength of steel and tensile strength reduce, but when inclusion particle is less than 0.3 μm, yield strength and tensile strength all will improve.
Calcium treatment is widely adopted at present and carries out modification to oxide inclusion in steel, and it is to Al in modified steel
2o
3be mingled with, improving steel performance has effect to a certain degree, but is also faced with some difficulties simultaneously.Such as, the vapour pressure of calcium is very high, and the solubleness in molten steel is very little; The oxide inclusion of calcium-base alloy modified aluminium, its modified product obtained not easily is removed, and when forming liquid phase in the periphery of inclusion particle, hinders the carrying out of reaction of degeneration, the product C aOAl that modification simultaneously obtains
2o
3not yielding, can tiny crack be formed at high-level rigid line in the cold drawn or operation of rolling, cause the penalty of steel.
Summary of the invention
Based on above-mentioned deficiency, the invention provides a kind of smelting process of Clean Steel of new nano particle dispersion-strengthened.The method can not only carry out inclusion conditioning to steel, and macrobead can also be removed in theory completely and be mingled with, retain a small amount of small-particle oxide particle, small-particle oxide compound size can control in 10 nanometers and following magnitude thereof, become strengthening phase in steel, be conducive to improving ferrous materials mechanical property.
The present invention adopts following technical scheme:
A smelting process for nano particle dispersion-strengthened steel, comprises the steps:
S100: will treat that the material of melting is placed in melting container, then described melting container is placed in magnetic levitation stove to carry out melting process and obtain molten steel, described in described melting process, the temperature of magnetic levitation stove is more than 1500 DEG C, and smelting time is more than or equal to 0.5 minute; Wherein saidly treat containing large inclusions in the material of melting, and described in treat in the material of melting containing titanium;
S200: carry out cooling to described molten steel and can obtain nano particle dispersion-strengthened steel, rate of cooling is included in the quick cooling of more than 1 centigrade per minute.
Wherein, treat that the material of melting is steel sample, containing titanium and iron in described steel sample described in.
Wherein, treat that the material of melting is the mixture of original steel sample and titanium, containing iron in described original steel sample described in.
Wherein, described in the material treating melting described in, the mass percentage of titanium is more than or equal to 0.1%.
Wherein, the titanium treating in the material of melting described in is the mixture of any one or the two in pure metal titanium and its alloys.
Wherein, described in treat also to comprise reductor in the material of melting, described reductor is that one in alkaline-earth metal, aluminium, titanium or its alloy mix corresponding oxide compound.
Wherein, the described melting process in step S100 is carried out under the protection of rare gas element or in vacuum.
Wherein, the magnetic suspension force of described magnetic levitation stove can make large inclusions in described molten steel at the float downward of magnetic field and molten steel buoyancy;
The step that the induced current of described magnetic levitation stove is regulated also is comprised in step S200.
Wherein, the cooling in step S200 comprises the quick cooling of rate of cooling more than 1 centigrade per minute;
Wherein, storing step S300 is also comprised after step S200:
S300: store under described nano particle dispersion-strengthened steel is placed in vacuum or protection of inert gas.
Wherein, the storing temp of the dispersion-strengthened steel of nano particle described in step S300 is for being less than 100 DEG C.
The invention has the beneficial effects as follows:
1. present invention achieves and use smelting process to obtain the dispersed particle-strengthened super-steel of nanometer scale (10 nm), for the technical scale volume production of oxide dispersion intensifying (Oxide dispersion strengthen (ODS)) steel provides a kind of new viable process, greatly can improve the production efficiency of ODS steel, reduce the production cost of ODS steel.
2. the present invention can effectively control cost, and by using magnetic levitation stove to add titanium and titanium alloys melting, can greatly reduce Al in steel
2o
3deng the quantity that related oxides is mingled with; And modification is carried out to the pattern of steel.While macrobead is mingled with removal, define the oxide particle of a large amount of nano level Dispersed precipitate, size can reach 10 nanometer scale; The refinement tissue of steel, improves the mechanical property of steel.
3. send out and have employed magnetic levitation stove and carry out melting, have feature rapidly and efficiently, in fusion process, molten steel is suspended state, avoids the pollution to molten steel that sidewall of crucible may cause.Molten steel along with strong rotation and stirring, more easily promotes that the floating of steel inclusion is removed at fusion process.
4. melting speed of the present invention is fast, and system is simple, and security is high, workable.
Accompanying drawing explanation
Fig. 1 is the SEM shape appearance figure of comparative example one;
Fig. 2 is the SEM shape appearance figure of comparative example two;
Fig. 3 is the SEM shape appearance figure of comparative example three
Fig. 4 is the SEM shape appearance figure of an embodiment of the smelting process of the Clean Steel adopting nano particle dispersion-strengthened of the present invention.
Fig. 5 is the TEM shape appearance figure that electrolysis adopts an embodiment of the smelting process of the Clean Steel of nano particle dispersion-strengthened of the present invention.
Fig. 6-Fig. 7 is the inclusion EDS collection of illustrative plates using pure iron melting.
Fig. 8-Fig. 9 is the EDS collection of illustrative plates of an embodiment of the smelting process of the Clean Steel adopting nano particle dispersion-strengthened of the present invention.
Embodiment
The present invention is described in detail below in conjunction with embodiment and accompanying drawing.It should be noted that, when not conflicting, the embodiment in the application and the feature in embodiment can combine mutually.
The invention provides a kind of smelting process of nano particle dispersion-strengthened steel, comprise the steps:
S100: will treat that the material of melting is placed in melting container, then described melting container is placed in magnetic levitation stove to carry out melting and obtain molten steel, the temperature of the stove of magnetic levitation described in fusion process is more than 1500 DEG C, and smelting time is more than or equal to 1 minute, and preferably smelting time is 1 ~ 10 minute.Wherein saidly treat containing large inclusions in the material of melting, and described in treat in the material of melting containing titanium.In this step, the temperature of magnetic levitation stove should be enough to make this original steel sample fusing form molten steel.The nano particle disperse that it should be noted that in the present embodiment refers to removes the micron-sized large inclusions contained in steel or disperse, and nano level particle is retained, and in follow-up process of cooling also not agglomeration, becomes the nano level strengthening phase in steel.In this step, the magnetic suspension force of magnetic levitation stove should be enough large thus make large inclusions in described molten steel at the float downward of magnetic field and molten steel buoyancy.Large inclusions in this step refers to the inclusion being greater than 1 micron dimension.Wherein composition of inclusions is depending on the amount of the reductor that adds and titanium and ratio, and may be a kind of oxide compound, also can be the eutectic product of several oxide compounds.
S200: carry out cooling to described molten steel after melting completes and can obtain nano particle dispersion-strengthened steel, the cold rate of cooling crossed in process is more than or equal to 1 DEG C/min.It should be noted that, cooling can be air cooling, also can be quench cooled in a liquid.Further, process of cooling can be carried out under the protection of rare gas element, a kind of type of cooling be cooled under molten steel being placed on protection of inert gas no longer rubescent after carry out water-cooled again.
S300: store under described nano particle dispersion-strengthened steel is placed in vacuum or protection of inert gas.Storing temp in this step is 20 DEG C-50 DEG C.Vacuum in this step refers to that oxygen content is less than 0.1 Pa.
The present embodiment have employed magnetic levitation stove to be added titanium simultaneously and carries out inclusion conditioning to steel, this melting method can remove the small-particle that macrobead retains tracer level, micron, the quantity of submicron order inclusion, size, distribution in effective minimizing steel, obtain the combined oxidation particle of nano level Dispersed precipitate, and the combined oxidation particle of nano level Dispersed precipitate as strengthening phase in steel, can improve every mechanical property of steel.
Wherein, treat that the material of melting is steel sample, containing titanium and iron in described steel sample described in.Namely the material putting into melting container such as crucible can be adopt iron powder, Al in advance
2o
3the steel sample of rear compacting is mixed with titanium.
As another kind of embodiment, described in treat that the material of melting is the mixture of original steel sample and titanium, containing iron in described original steel sample.Original steel sample in the present embodiment is iron powder and Al
2o
3mix the steel sample of rear compacting, that is shaping steel sample.Therefore, method of the present invention had both gone for the fusion process of steel sample, also may be used for the further process to steel sample.
The titanium treating in the material of melting in step S100 can be pure metallic titanium or titanium alloy or the mixture of the two, as long as ensure to treat that the titanium content in the material of melting is more than or equal to 0.1%.When adopting titanium alloy, preferred titaniferous amount is the titanium alloy of more than 1%.
Preferably, as another kind of embodiment, described in treat also to comprise reductor in the material of melting, described reductor is that one in alkaline-earth metal, aluminium, titanium or its alloy mix corresponding oxide compound.The content of reductor can be any.The best aluminium of described reductor (Al) or aluminium (Al) and aluminum oxide (Al
2o
3) mixture.Wherein aluminium (Al) and aluminum oxide (Al
2o
3) mixture in the ratio of aluminium and aluminum oxide can be any ratio.Preferably, the mass ratio that aluminium accounts for original steel sample is 0.1 ~ 15g/kg, and the mass ratio that aluminum oxide accounts for original steel sample is 0.1 ~ 15g/kg.
Preferably, as a kind of embodiment, described fusion process carries out under the protection of rare gas element or in a vacuum.Rare gas element can be passed into or by magnetic levitation stove vacuum state in magnetic levitation stove in the present embodiment.The oxygen in molten steel absorption air can be avoided like this, form more oxide inclusion.Wherein said rare gas element is argon gas, helium, neon or xenon.
Wherein, described process of cooling be specially described molten steel is cooled in described magnetic levitation stove there is no red heat after take out again and carry out water-cooled.Preferably, the process of cooling occurred in magnetic levitation stove is also carried out under the protection of rare gas element.
Preferably, as a kind of embodiment, the magnetic suspension force of described magnetic levitation stove can make large inclusions in described molten steel at the float downward of magnetic field and molten steel buoyancy.The magnetic suspension force of the magnetic levitation stove namely used in this step should be enough large thus make large inclusions in described molten steel at the float downward of magnetic field and molten steel buoyancy.Large inclusions in this step refers to the inclusion being greater than 1 micron.
Further, the step that the induced current of described magnetic levitation stove is regulated also is comprised in step S200.By the stirring regulating the induced current in magnetic levitation stove can strengthen molten steel, molten steel acutely overturns in crucible, reduces the size of steel inclusion, and the floating further promoting steel inclusion is removed.
Below with Al
2o
3inclusion is that the present invention is further described for example.
Comparative example 1
Comparative example 1 is the experiment that independent melting pure iron probes into inclusion size, pattern.
Concrete operation step is as follows:
S100: straight iron powder briquetting is obtained original steel sample.Straight iron powder in this step adopts atomized iron powder, and composition is by weight percentage, and Fe content reaches more than 99%.
S200: be placed in crucible by original steel sample, crucible is placed in magnetic levitation stove and carries out melting and obtain molten steel, the temperature of the stove of magnetic levitation described in fusion process is more than 1500 DEG C, and smelting time is 4 minutes.Melting is carried out under an argon atmosphere.
S300: carry out cooling to described molten steel after melting completes and obtain the first steel sample, the cold rate of cooling crossed in process is 1 DEG C/min.
The first steel sample warp melting obtained cuts into square fritter, observes specimen holder foreign material size, pattern and distribution situation after polish etch under scanning electron microscope.The polished surface inclusion SEM of comparative example 1 schemes as shown in Figure 1, and as can be seen from Figure 1, there is more Spherical Inhomogeneity in steel, inclusion size is between 1-3 μm.Carry out deoxidation owing to not adding reductor in sample, so the inclusion in steel mainly exists with the oxide form of iron, the oxide compound of these iron will reduce fatigue strength and the impelling strength of steel.
Comparative example 2
Comparative example 2 is in straight iron powder, add conventional reductor Al and typical inclusion Al
2o
3the experiment of melting.Wherein Al and Al
2o
3use analytical reagent.
Concrete operation step is as follows:
S100: by Al, Al
2o
3after straight iron powder grinding evenly, then briquetting obtains original steel sample.Straight iron powder in this step adopts atomized iron powder, and composition is by weight percentage, and Fe content reaches more than 99%.Wherein the mass percentage of Al is 3%, Al
2o
3mass percentage be 3%.
S200: be placed in crucible by original steel sample, crucible is placed in magnetic levitation stove and carries out melting and obtain molten steel, the temperature of the stove of magnetic levitation described in fusion process is more than 1500 DEG C, and smelting time is 4 minutes.Melting is carried out under an argon atmosphere.
S300: carry out cooling to described molten steel after melting completes and obtain the second steel sample, the cold rate of cooling crossed in process is 1 DEG C/min.
The second steel sample warp that melting obtains cuts into square fritter, observes specimen holder foreign material size, pattern and distribution situation after polish etch under scanning electron microscope.The polished surface inclusion SEM of comparative example 2 schemes as shown in Figure 2, as can be seen from Figure 2, owing to adding quantitative Al in sample
2o
3, there is a large amount of Spherical Inhomogeneity in steel, these inclusiones be mainly Al
2o
3particle, size is between 0.5-2.5 μm.Due to dystectic Al
2o
3particle is still solid-state in molten steel, works as Al
2o
3when size is greater than 1 μm, the yield strength of steel and tensile strength is influenced will reduce; Work as Al
2o
3when size is less than 0.3 μm, the yield strength of steel and tensile strength can strengthen on the contrary to some extent.
Comparative example 3
Comparative example 3 is the experiment adding titanium melting in straight iron powder.
Concrete operation step is as follows:
S100: after pure metallic titanium and straight iron powder grinding evenly, then briquetting obtains original steel sample.Straight iron powder in this step adopts atomized iron powder, and composition is by weight percentage, and Fe content reaches more than 99%.Wherein the mass percentage of pure metallic titanium is 6%.
S200: be placed in crucible by original steel sample, crucible is placed in magnetic levitation stove and carries out melting and obtain molten steel, the temperature of the stove of magnetic levitation described in fusion process is more than 1500 DEG C, and smelting time is 4 minutes.Melting is carried out under an argon atmosphere.
S300: carry out cooling to described molten steel after melting completes and obtain the 3rd steel sample, the cold rate of cooling crossed in process is 1 DEG C/min.
The polished surface inclusion SEM of the 3rd steel sample schemes as shown in Figure 3, as can be seen from Figure 3, adds deoxidation properties-correcting agent Ti-Fe, can reduce oxygen content in steel in sample, obtains the oxide particle of small and dispersed distribution.Still remained part inclusion in steel, size is between 0.5-1 μm.The performance of existence on steel of these inclusiones still has impact to a certain extent, does not reach the sublimate desired by us and the result of nano particle dispersion-strengthened.
Embodiment 1
Embodiment 1 for add deoxidation properties-correcting agent Ti in straight iron powder, reductor Al and typical inclusion Al
2o
3the experiment of melting.
Concrete operation step is as follows:
S100: by Al, Al
2o
3, after titanium-iron powder and straight iron powder grinding evenly, then briquetting obtains original steel sample.Straight iron powder in this step adopts atomized iron powder, and composition is by weight percentage, and Fe content reaches more than 99%.Wherein the mass percentage of titanium-iron powder is 5%, and in the present embodiment, the mass percentage of Al is 3%, Al
2o
3mass percentage be 3%.
S200: be placed in crucible by original steel sample, crucible is placed in magnetic levitation stove and carries out melting and obtain molten steel, the temperature of the stove of magnetic levitation described in fusion process is more than 1500 DEG C, and smelting time is 4 minutes.Melting is carried out under an argon atmosphere.
S300: carry out cooling to described molten steel after melting completes and obtain the 4th steel sample, the cold rate of cooling crossed in process is 1 DEG C/min.
Polished surface inclusion SEM schemes as shown in Figure 4, and as can be seen from Figure 4, comparison diagram 2, in sample, the amount of inclusions obviously reduces, and only finds the inclusion particle of minute quantity in field range.These are mingled with the mixture being mainly Ti-Al-O-Fe, and because the amount of inclusions is less, size is tiny, so they can be ignored on the impact of steel performance.This result indicates the feasibility that sublimate is smelted.Simultaneously due to the limitation of scanning electron microscope, the inclusion particle of nano level Dispersed precipitate may be there is in sample, but do not observe the pattern of these particles by SEM picture, observe so make transmission electron microscope (TEM) sample by the electrolytic process inclusion reclaimed in steel sample.As can be seen from Figure 5, really there is nanometer Particulate Inclusion in steel, size is at 5-40nm.Contrast (Fig. 6-Fig. 7) and (Fig. 8-Fig. 9) can be found out, these nano particles are mainly the mixture of Fe-O-S-Al-Ti.The existence of these nano particles, not only can not reduce the performance of steel, has extremely strong promoter action on the contrary to the raising of steel mechanics performance.Therefore, by this experimental technique, substantially reach the object that sublimate is smelted, obtain the nanometer Particulate Inclusion of Dispersed precipitate in steel simultaneously, substantially increase steel performance, and provide a kind of effective means for obtaining ODS steel by smelting method.
Ti-Fe melting and the amount of inclusions and the distribution of sizes situation that do not add Ti-Fe melting is added in table 1:SEM figure
The present invention adopts containing Al
2o
3steel in add the method for Ti additive by the melting of magnetic levitation stove, the quantity of steel inclusion is obviously reduced, inclusion size reduces greatly simultaneously, obtain the nanometer of Dispersed precipitate in steel to be mingled with, while realizing sublimate smelting, nano-inclusion can promote the raising of steel performance, obtains ODS steel provide a kind of feasible technique for adopting melting method.It should be noted that method provided by the invention both went for smelting steel, also can the steel smelted be processed further simultaneously.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (11)
1. a smelting process for nano particle dispersion-strengthened steel, is characterized in that, comprises the steps:
S100: will treat that the material of melting is placed in melting container, then described melting container is placed in magnetic levitation stove to carry out melting process and obtain molten steel, described in described melting process, the temperature of magnetic levitation stove is more than 1500 DEG C, and smelting time is more than or equal to 0.5 minute; Wherein saidly treat containing large inclusions in the material of melting, and described in treat in the material of melting containing titanium;
S200: cooling is carried out to described molten steel and can obtain nano particle dispersion-strengthened steel.
2. method according to claim 1, is characterized in that, described in treat that the material of melting is steel sample, containing titanium and iron in described steel sample.
3. method according to claim 1, is characterized in that, described in treat that the material of melting is the mixture of original steel sample and titanium, containing iron in described original steel sample.
4. method according to claim 1, is characterized in that, described in treat melting material described in the mass percentage of titanium be more than or equal to 0.1%.
5. method according to claim 1, is characterized in that, described in treat in the material of melting titanium and be the mixture of any one or the two in pure metal titanium and its alloys.
6. method according to claim 1, is characterized in that, described in treat also to comprise reductor in the material of melting, described reductor is that one in alkaline-earth metal, aluminium, titanium or its alloy mix corresponding oxide compound.
7. method according to claim 1, is characterized in that, the described melting process in step S100 is carried out under the protection of rare gas element or in vacuum.
8. method according to claim 1, is characterized in that, the magnetic suspension force of described magnetic levitation stove can make large inclusions in described molten steel at the float downward of magnetic field and molten steel buoyancy;
The step that the induced current of described magnetic levitation stove is regulated also is comprised in step S200.
9. method according to claim 1, is characterized in that, the rate of cooling in step S200 is more than 1 centigrade per minute.
10. method according to claim 1, is characterized in that, also comprises storing step S300 after step S200:
S300: store under described nano particle dispersion-strengthened steel is placed in vacuum or protection of inert gas.
11. methods according to claim 10, is characterized in that, the storing temp of the dispersion-strengthened steel of nano particle described in step S300 is for being less than 100 DEG C.
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