CN104858444A - Hypoxic manganese-containing water atomized steel powder reduction process - Google Patents
Hypoxic manganese-containing water atomized steel powder reduction process Download PDFInfo
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- CN104858444A CN104858444A CN201510318414.3A CN201510318414A CN104858444A CN 104858444 A CN104858444 A CN 104858444A CN 201510318414 A CN201510318414 A CN 201510318414A CN 104858444 A CN104858444 A CN 104858444A
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Abstract
The invention discloses a hypoxic manganese-containing water atomized steel powder reduction process. A high-temperature reduction method is adopted to reduce water atomized FeMn powder, the room temperature is improved to be low-temperature reduction temperature, the low-temperature reduction temperature is kept for certain time and then is improved to be high-temperature reduction temperature, and the high-temperature reduction temperature is kept for certain time. The low-temperature reduction temperature is 550-750 DEG C and is kept for 0.5-2 hours. The high-temperature reduction temperature is 900-1000 DEG C and is kept for 1-2 hours. The reduction process include two stages, wherein at the low-temperature stage, the low-temperature reduction time is properly increased to reduce an iron oxide, remove more oxygen, decrease a manganese oxide to the greatest extent and reduce manganese oxidation and transfer at the high-temperature stage. Compared with pure 970 DEG C annealing and reduction, the two-stage method enables the powder surface oxygen content to be decreased obviously, the total oxygen content is also reduced to be lower than 0.2%, and compared with pure 970 DEG C annealing and reduction, the oxygen content is reduced by 61%.
Description
Technical field
That the present invention relates to is the preparation method of water atomised iron-based powder.More specifically, the present invention relates to the reducing process of the manganese containing water atomization comminuted steel shot producing hypoxemia.
Background technology
Manganese is the base alloy elements of high-tensile structural steel and austenitic manganese steel.In field of powder metallurgy, manganese possesses higher strengthening ability, and its cost is far below other alloying element.Water atomization pulverization has output greatly simultaneously, and the feature that cost is low, belongs to the main technology of preparing of Powder Metallurgy Industry.Manganese has three kinds of incorporation way as alloying element: element powders method, foundry alloy method and atomization.Water atomization is a kind of low cost technology of preparing containing manganese low-alloy steel powder, its principle adds the alloying elements such as Mn in ferrous metals melts, after abundant alloying, applying high voltage current directly smash aluminium alloy stream (being namely atomized), the fecula obtained again through the Reduction of Oxide of high temperature by powder surface, thus obtains that purity is higher, the uniform comminuted steel shot of alloying elements distribution.
Oxygen content is the important performance indications of steel powder, is subject to the attention of Powder Metallurgy Industry always.Oxide generally can increase powder hardness, infringement suppression performance, the percentage elongation reducing agglomerated material and toughness.For containing manganese low-alloy steel material, sintering process once formation network will hinder densified, significantly reduces material property containing Mn oxide.Because manganese element oxytropism is strong, powder surface oxidation is the main cause hindering the development of manganese containing water atomization prealloy comminuted steel shot.
Powder has higher specific area, in water atomization and follow-up technique, inevitably causes the oxidation of powder, without the water atomization including Mn-Fe powder oxygen content of reducing between 0.4%-1%, there are some researches show the oxide that its major part is iron.For reducing oxygen content to the adverse effect of suppressing and sinter, need to carry out reduced anneal to powder.Because manganese is oxidizable, more difficult reduction, when 1200 DEG C is not
hydrogenreduction, can be reduced by carbon during 1100-1200 DEG C.The oxidation of manganese is easily formed in reduced anneal process.The oxidation of manganese derives from two aspects: one is the water in reducing atmosphere, reducing atmosphere can not reach in actual industrial 100% pure, containing trace water also can cause oxidation to manganese; Two is that the oxide of manganese and iron reacts, and forms oxidation transfer.The dew point of current industrial application reducing atmosphere is usually below-50 DEG C, and far below the oxygen content of 0.4%-1% in water-atomized iron powder, therefore in reduced anneal, the oxidation of manganese is mainly derived from oxidation transfer.Prevent the oxidation transfer of manganese in reduction sintering from being prepare the key issue that manganese containing water atomized iron powder need solve.
Water atomization is mainly ferriferous oxide and the more stable Mn oxide of thermodynamics containing the composition of manganese prealloy comminuted steel shot reduction rear surface oxide, and wherein Mn oxide mainly exists with the form on " oxygen island ".Ferriferous oxide can reduce in the nitrogen atmosphere of low temperature.But Mn oxide can only be reduced by carbon, and can not reduce by hydrogen.After sintering, Mn oxide is still present on particle and granuloplastic neck interface, hinders the connection between particle.Therefore to have good sinterability energy containing manganese sintered steel structural member, just necessarily require the coverage rate on powder surface oxygen island lower than 10%.
A lot of result of study shows, due to Mn oxide and ferriferous oxide thermodynamics is non-equilibrium and the increase of diffusion rate, making to be oxidized the transfer the most dangerous stage containing carrying out in manganese metallic sintered products heating process between 800 DEG C-1000 DEG C, therefore should avoid as far as possible in this interval heating for a long time.
Sweden He Jianaisi discloses the preparation technology of " powder of stainless steel ", which employs at least at the annealing process of 1120 DEG C.But annealing will make powder seriously lump more than 1120 DEG C, greatly increase the broken difficulty of subsequent technique, force fragmentation also easily to make powder form work hardening, reduce the compressible performance of powder.Therefore the highest reduced anneal temperature that enterprise adopts usually to water-atomized iron powder is 970 DEG C.As mentioned above, 970 DEG C are in and are formed within the most dangerous temperature range of oxidation transfer containing manganese alloy comminuted steel shot, and with the increase of Fe content in powder, after reduction, the coverage rate on powder surface oxygen island also can increase fast, therefore can only prepare the very low iron-based powder of Fe content.
In water atomization process, high temperature liquid iron and water generation oxidation reaction, form oxide layer at powder surface, there are some researches show that its major part is the oxide of iron.Ferriferous oxide is easy to by hydrogen reducing below 800 DEG C.In order to avoid oxidation transfer dangerous temperature scope, below 800 DEG C, manganese containing water atomized iron powder is reduced, but effect is unsatisfactory.Trace it to its cause, manganese is solid-solution in high temperature liquid iron, with water generation oxidation reaction, due to water atomization process cooling velocity quickly, the reaction time is short, and Mn oxide and ferriferous oxide are difficult to form the phase be separated, and the oxidation state of powder surface is also still solid solution state.The solid solution of Mn oxide in ferriferous oxide adds the reduction difficulty of ferriferous oxide, and with the reduction of iron oxide in oxide layer, the content of the Mn oxide in surface oxide layer can increase further.From reduction thermodynamics, now or further improve reduction temperature, or reduce the content of steam in reducing gas further.Industrially be difficult to the dew point reducing reducing gas further, therefore must improve the further reduction that reduction temperature just can impel surface oxide layer, and improve reduction temperature and can bring following process difficulty (as mentioned above).Therefore, an ideal technique is not also found can to prepare the Fe content water atomization comminuted steel shot that more elevated oxygen level is lower at present.
Summary of the invention
For prior art above shortcomings, the object of the present invention is to provide a kind of hypoxemia manganese containing water to be atomized the reducing process of comminuted steel shot, the present invention can prepare the Fe content water atomization comminuted steel shot that more elevated oxygen level is lower.
For solving the problems of the technologies described above, realize goal of the invention, the technical solution used in the present invention is as follows:
A kind of reducing process of hypoxemia manganese containing water atomization comminuted steel shot, high temperature reduction method is adopted to reduce to water atomization FeMn fecula, high temperature reduction temperature is 900-1000 DEG C, it is characterized in that: adopt two step reducing process, first rise to low-temperature reduction temperature from room temperature, at low-temperature reduction temperature, be raised to high temperature reduction temperature again and held for some time after held for some time, be cooled to less than 500 DEG C with stove after insulation terminates, then be pushed into water-cooled district cool to room temperature; Wherein low-temperature reduction temperature is 550-750 DEG C, and temperature retention time is 0.5-2h; The high temperature reduction temperature time is 1-2h.
Further, the heating rate rising to low-temperature reduction temperature from room temperature is 4-15 DEG C/min; The heating rate being raised to high temperature reduction temperature from low-temperature reduction temperature is 4-20 DEG C/min.
Wherein reducing atmosphere is H
2atmosphere, dew point is not higher than-40 DEG C.
Preferred low-temperature reduction temperature is 650 DEG C, insulation 45min; High temperature reduction temperature is 970 DEG C, insulation 1h.
Compared to prior art, tool of the present invention has the following advantages:
Present invention employs two benches reducing process, the cold stage in temperature-rise period, suitably increase the low-temperature reduction time, ferriferous oxide is reduced, removes more oxygen, and reduce the formation of Mn oxide as far as possible, to reduce the oxidation transfer of hot stage manganese.With merely compared with 970 DEG C of reduction of anneal, two-phase method can make powder surface Yang Island content obviously decline, and total oxygen content is also reduced to less than 0.2%, and compared with simple 970 DEG C reduction of annealing, oxygen content reduction amplitude reaches 61%.
Adopt water atomization and two step reduction method to combine, effectively can suppress the formation of netted oxide, obtain alloying elements distribution uniform FeMn prealloy comminuted steel shot.When Fe content is 2.0wt.%, sintered part mechanical property is best, and hot strength is 681MPa, compares and exceeds 7.4%, and percentage elongation is 3.22%.
Detailed description of the invention
The reducing process of hypoxemia manganese containing water atomization comminuted steel shot of the present invention, adopt high temperature reduction method to reduce to water atomization FeMn fecula, prior art is directly warmed up to high temperature reduction temperature, and high temperature reduction temperature is generally 900-1000 DEG C.The present invention adopts two step reduction method, namely first low-temperature reduction temperature is risen to from room temperature, high temperature reduction temperature is raised to again and held for some time after held for some time at low-temperature reduction temperature, 500 DEG C of annealing are cooled to stove after insulation terminates, be pushed into water-cooled district cool to room temperature again, after crushing and screening, obtain reduced powder.Wherein low-temperature reduction temperature is 550-750 DEG C, and temperature retention time is 0.5-2h; The high temperature reduction temperature time is 1-2h.Preferred low-temperature reduction temperature is 600-700 DEG C, and temperature retention time is 0.5-1h; More preferably 650 DEG C, insulation 45min.The preferred 930-980 DEG C of high temperature reduction temperature, insulation 1.5-2h, more preferably 970 DEG C, insulation 2h.The reducing atmosphere of reduction process is H
2atmosphere, gas flow 2L/min, dew point is not higher than-40 DEG C.
During actual intensification, the heating rate rising to low-temperature reduction temperature from room temperature is 4-15 DEG C/min; The heating rate being raised to high temperature reduction temperature from low-temperature reduction temperature is 4-20 DEG C/min.Preferably, the heating rate rising to low-temperature reduction temperature from room temperature is 5 DEG C/min; The heating rate being raised to high temperature reduction temperature from low-temperature reduction temperature is 5 DEG C/min.
Below in conjunction with comparative example, the present invention and effect thereof are described in further detail.
When specifically carrying out contrast test, choose the water atomization low-alloy fecula that Fe content is 2.5wt.%, design four groups of different reducing process and be analyzed, its heating schedule is respectively: A1-5 DEG C/min rises to 970 DEG C, insulation 2h; A2-5 DEG C/min rises to 650 DEG C, insulation 2h; A3-5 DEG C/min rises to 650 DEG C, and after insulation 45min, then 5 DEG C/min rises to 970 DEG C, insulation 2h; A4-5 DEG C/min rises to 650 DEG C, and after insulation 2h, then 5 DEG C/min rises to 970 DEG C, insulation 2h.Each group of test is all at H
2reduce in atmosphere, dew point of atmosphere-35 DEG C, gas flow 2L/min.Be cooled to 500 DEG C with stove after insulation terminates, then be pushed into water-cooled district cool to room temperature.
After different process reduction, the essential element content of powder is as shown in table 1, and the Fe-2.5Mn alloy fecula oxygen content without reduction is 3.29%.Programming rate is 5 DEG C/min, and after 970 DEG C of insulation reductase 12 h, the oxygen content of powder has been reduced to 0.36%.
The constituent content of table 1 Fe-2.5Mn fecula powder after different process reduction
| Mn(wt.%) | C(wt.%) | O(wt.%) | |
| Fecula | 2.49 | 0.057 | 3.29 |
| A1 | 2.45 | 0.012 | 0.36 |
| A2 | 2.49 | 0.018 | 0.49 |
| A3 | 2.48 | 0.012 | 0.16 |
| A4 | 2.46 | 0.011 | 0.26 |
Powder will have good compressibility and sintering character, and General Requirements powder total oxygen content lower than 0.2%, will adopt A1 technique to be directly warming up to 970 DEG C of reduction Fe-2.5Mn by table 1 and be difficult to reach technical requirement as seen.Adopt A2 technique, at 650 DEG C of insulation reductase 12 h, because reduction temperature is low, can only reduce part iron and manganese oxides, powder total oxygen content, up to 0.49%, more difficultly reaches technical requirement.Adopt A3, A4 technique, be incubated reduction in two stages, effectively can reduce the total oxygen content of powder.Particularly A3 technique, after 650 DEG C of insulation reduction 45min, then rises to 970 DEG C of insulation reductase 12 h, powder total oxygen content can be made to be reduced to 0.16%, can meet the requirement of technical indicator to oxygen content.In A4 technique, after 650 DEG C of holding times to 2h, the total oxygen content of powder has rising again, reaches 0.26%.Therefore, technique A3 can prepare and guarantees that Fe content level does not reduce the lower water atomization comminuted steel shot of oxygen content under prerequisite.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (4)
1. the reducing process of a hypoxemia manganese containing water atomization comminuted steel shot, high temperature reduction method is adopted to reduce to water atomization FeMn fecula, high temperature reduction temperature is 900-1000 DEG C, it is characterized in that: adopt two step reducing process, first rise to low-temperature reduction temperature from room temperature, at low-temperature reduction temperature, be raised to high temperature reduction temperature again and held for some time after held for some time, be cooled to less than 500 DEG C with stove after insulation terminates, then be pushed into water-cooled district cool to room temperature; Wherein low-temperature reduction temperature is 550-750 DEG C, and temperature retention time is 0.5-2h; The high temperature reduction temperature time is 1-2h.
2. the reducing process of hypoxemia manganese containing water atomization comminuted steel shot as claimed in claim 1, is characterized in that: the heating rate rising to low-temperature reduction temperature from room temperature is 4-15 DEG C/min; The heating rate being raised to high temperature reduction temperature from low-temperature reduction temperature is 4-20 DEG C/min.
3. the reducing process of hypoxemia manganese containing water atomization comminuted steel shot as claimed in claim 1, is characterized in that: reducing atmosphere is H
2atmosphere, dew point is not higher than-40 DEG C.
4. the reducing process of hypoxemia manganese containing water atomization comminuted steel shot as claimed in claim 1, is characterized in that: preferred low-temperature reduction temperature is 650 DEG C, insulation 45min; High temperature reduction temperature is 970 DEG C, insulation 1h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104858444B (en) * | 2015-06-11 | 2017-04-26 | 四川理工学院 | Hypoxic manganese-containing water atomized steel powder reduction process |
| CN106694871A (en) * | 2017-02-28 | 2017-05-24 | 四川理工学院 | Method for improving compactibility of manganese-containing steel powder |
| CN106735307A (en) * | 2017-02-28 | 2017-05-31 | 四川理工学院 | Water atomization prealloy containing manganese comminuted steel shot oxygen content regulates and controls method |
| CN112267003A (en) * | 2020-09-24 | 2021-01-26 | 山东鲁银新材料科技有限公司 | Preparation method of water atomized pure iron powder with ultrahigh cleanliness, low oxygen and high performance |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104858444B (en) * | 2015-06-11 | 2017-04-26 | 四川理工学院 | Hypoxic manganese-containing water atomized steel powder reduction process |
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2015
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Patent Citations (7)
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| JPH01290703A (en) * | 1988-05-16 | 1989-11-22 | Daido Steel Co Ltd | Kneaded matter of low-alloy steel powder for sintering |
| JPH0517801A (en) * | 1991-07-10 | 1993-01-26 | Kobe Steel Ltd | Production of diffusion type low-alloy steel powder having excellent compressibility |
| JPH1096001A (en) * | 1996-08-02 | 1998-04-14 | Kawasaki Steel Corp | Production of partially diffused alloyed steel powder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104858444B (en) * | 2015-06-11 | 2017-04-26 | 四川理工学院 | Hypoxic manganese-containing water atomized steel powder reduction process |
| CN106694871A (en) * | 2017-02-28 | 2017-05-24 | 四川理工学院 | Method for improving compactibility of manganese-containing steel powder |
| CN106735307A (en) * | 2017-02-28 | 2017-05-31 | 四川理工学院 | Water atomization prealloy containing manganese comminuted steel shot oxygen content regulates and controls method |
| CN106735307B (en) * | 2017-02-28 | 2018-08-17 | 四川理工学院 | The water atomization comminuted steel shot oxygen content of prealloy containing manganese regulates and controls method |
| CN112267003A (en) * | 2020-09-24 | 2021-01-26 | 山东鲁银新材料科技有限公司 | Preparation method of water atomized pure iron powder with ultrahigh cleanliness, low oxygen and high performance |
| CN112267003B (en) * | 2020-09-24 | 2022-05-03 | 山东鲁银新材料科技有限公司 | Preparation method of water atomized pure iron powder with ultrahigh cleanliness, low oxygen and high performance |
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