CN104858444B - 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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- CN104858444B CN104858444B CN201510318414.3A CN201510318414A CN104858444B CN 104858444 B CN104858444 B CN 104858444B CN 201510318414 A CN201510318414 A CN 201510318414A CN 104858444 B CN104858444 B CN 104858444B
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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
The present invention relates to the preparation method of water atomised iron-based powder.More particularly it relates to produce hypoxia
Manganese containing water is atomized the reducing process of comminuted steel shot.
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
Reinforcing ability, and its cost be far below other alloying elements.Simultaneously water atomization pulverization has yield big, the characteristics of low cost,
Belong to the main technology of preparing of Powder Metallurgy Industry.Manganese has three kinds of incorporation ways as alloying element：Element powders method, foundry alloy
Method and atomization.Water atomization is a kind of inexpensive technology of preparing of the powder of low-alloy steel containing manganese, and its principle is in ferrous metals melts
The alloying elements such as middle addition Mn, directly smash aluminium alloy stream using High-Pressure Water after abundant alloying（It is atomized）, the life for obtaining
The oxide on powder surface is reduced by powder again through high temperature, and so as to obtain, purity is higher, the uniform comminuted steel shot of alloying elements distribution.
Oxygen content is the important performance indications of steel powder, is constantly subjected to the attention of Powder Metallurgy Industry.Oxide is general
Powder hardness, infringement suppression performance, the elongation percentage and toughness that reduce sintered material can be increased.For the material of low-alloy steel containing manganese,
Sintering process is greatly reduced material property containing Mn oxide once forming network will hinder densification.Due to manganese element oxytropism
By force, powder surface oxidation is the main cause for hindering manganese containing water atomization prealloy comminuted steel shot development.
Powder has higher specific surface area, in water atomization and follow-up technique, inevitably causes powder
Oxidation, without reduction water atomization including Mn-Fe powder oxygen content between 0.4%-1%, there are some researches show its major part for ferrum oxygen
Compound.To reduce oxygen content to the adverse effect suppressed and sinter, need to carry out reduced anneal to powder.Because manganese is oxidizable,
More difficult reduction, when 1200 DEG C be notHydrogenReduction, can be reduced by carbon when 1100-1200 DEG C.Easily formed during reduced anneal
The oxidation of manganese.The oxidation of manganese derives from two aspects：One is the water in reducing atmosphere, and reducing atmosphere is impossible in actual industrial
Reach 100% it is pure, containing micro water also can to manganese cause oxidation；Two is that manganese is reacted with the oxide of ferrum, forms oxidation and turns
Move.Generally below -50 DEG C, the oxygen far below 0.4%-1% in water-atomized iron powder contains the dew point of industrial application reducing atmosphere at present
Amount, therefore the oxidation of manganese is mainly derived from oxidation transfer in reduced anneal.Prevent oxidation transfer of the manganese in reduction sintering from being system
The key issue that standby manganese containing water atomized iron powder need to be solved.
After the reduction of water atomization prealloy containing manganese comminuted steel shot, the composition of oxide on surface is mainly iron oxides and thermodynamics are more steady
Fixed Mn oxide, wherein Mn oxide are mainly in the form of " oxygen island ".Iron oxides can be in the nitrogen atmosphere of low temperature
Reduction.But Mn oxide can only be reduced by carbon, and can not be reduced by hydrogen.After sintering, Mn oxide is still present in granule
On granuloplastic cervical region interface, the connection between granule is hindered.Therefore the structural member of sintered steel containing manganese will have good
Sinterability energy, just necessarily require powder Surface Oxygen island coverage rate be less than 10%.
Many results of study show, as Mn oxide and iron oxides thermodynamics are non-equilibrium and the increasing of diffusion rate
Plus so that it is to carry out in the heating process of metallic sintered products containing manganese aoxidizing the transfer most dangerous stage between 800 DEG C -1000 DEG C,
Therefore the interval prolonged heating of here should be avoided as far as possible.
Sweden He Jianaisi is disclosed《Powder of stainless steel》Preparation technology, which employs the lehr attendant at least at 1120 DEG C
Skill.But in 1120 DEG C of broken difficulty that powder will be made seriously to lump, subsequent technique is greatly increased annealed above, force broken
Easily make powder form processing hardening, reduce the compressibility energy of powder.Therefore highest of the enterprise to the usual employing of water-atomized iron powder
Reduced anneal temperature is 970 DEG C.As described above, 970 DEG C form the most dangerous temperature model of oxidation transfer in comminuted steel shot containing manganese alloy
Within enclosing, with the increase of manganese content in powder, after reduction, the coverage rate on powder Surface Oxygen island also quickly can increase, therefore can only
Prepare the very low iron-based powder of manganese content.
During water atomization, there is oxidation reaction with water in high temperature liquid iron, forms oxide layer on powder surface, has research table
Oxide of bright its major part for ferrum.Iron oxides are easy to by hydrogen reducing below 800 DEG C.In order to avoid oxidation transfer danger
Dangerous temperature range, is reduced to manganese containing water atomized iron powder below 800 DEG C, but effect is unsatisfactory.Trace it to its cause, manganese
It is solid-solution in high temperature liquid iron, oxidation reaction occurs with water, as water atomization process rate of cooling is very fast, the response time is short, manganese
Oxide is difficult to form detached phase with iron oxides, and the oxidation state on powder surface is also still solid solution state.Mn oxide is in ferrum oxygen
Solid solution in compound increased the reduction difficulty of iron oxides, and with the reduction of ferrum oxide in oxide layer, in surface oxide layer
The content of Mn oxide further can increase.Knowable to reduction thermodynamics, or now further improving reduction temperature, or
The content of steam in reducing gas is reduced further.Industrially it is difficult to further reduce the dew point of reducing gas, it is therefore necessary to carry
High reduction temperature can just promote the further reduction of surface oxide layer, and improve reduction temperature and following process can be brought difficult
（As mentioned above）.Therefore, there is presently no and find an ideal technique can to prepare manganese content more elevated oxygen level lower
Water atomization comminuted steel shot.
The content of the invention
For deficiencies of the prior art, it is an object of the invention to provide a kind of hypoxia manganese containing water atomization comminuted steel shot
Reducing process, the present invention can prepare the lower water atomization comminuted steel shot of manganese content more elevated oxygen level.
To solve above-mentioned technical problem, goal of the invention is realized, the technical solution used in the present invention is as follows：
A kind of hypoxia manganese containing water is atomized the reducing process of comminuted steel shot, water atomization FeMn fecula is carried out also using high temperature reduction method
Original, high temperature reduction temperature are 900-1000 DEG C, it is characterised in that：Using two step reducing process, first low-temperature reduction is risen to from room temperature
Temperature, is raised again to high temperature reduction temperature held for some time at a temperature of low-temperature reduction after held for some time, insulation terminates
Furnace cooling is to less than 500 DEG C afterwards, then is pushed into water-cooled area and is cooled to room temperature；Wherein low-temperature reduction temperature is 550-750 DEG C, insulation
Time is 0.5-2h；The high temperature reduction temperature time is 1-2h.
Further, the heating rate for rising to low-temperature reduction temperature from room temperature is 4-15 DEG C/min；From low-temperature reduction temperature
The heating rate for being raised to high temperature reduction temperature is 4-20 DEG C/min.
Wherein reducing atmosphere is H2Atmosphere, not higher than -40 DEG C of dew point.
Preferred low-temperature reduction temperature is 650 DEG C, is incubated 45min；High temperature reduction temperature is 970 DEG C, is incubated 1h.
Compared to prior art, the invention has the advantages that：
Two benches reducing process is present invention employs, the cold stage in temperature-rise period, during appropriate increase low-temperature reduction
Between, iron oxides are reduced, more oxygen, and the formation of reduction Mn oxide as far as possible is removed, to reduce hot stage manganese
Oxidation transfer.Compared with reduction is annealed at 970 DEG C merely, two-phase method is decreased obviously can powder Biao Mian Yang Island contents, always
Oxygen content is also reduced to less than 0.2%, and compared with simple 970 DEG C are annealed reduction, oxygen content reduces amplitude up to 61%.
Combined using water atomization and two step reduction method, can effectively suppress the formation of netted oxide, obtain alloy unit
The FeMn prealloy comminuted steel shots that element is evenly distributed.When manganese content is 2.0wt.%, preferably, tensile strength is sintered part mechanical property
681MPa, compares and is higher by 7.4%, and elongation percentage is 3.22%.
Specific embodiment
Hypoxia manganese containing water of the present invention is atomized the reducing process of comminuted steel shot, water atomization FeMn fecula is carried out using high temperature reduction method
Reduction, prior art is directly to be warmed up to high temperature reduction temperature, and high temperature reduction temperature is usually 900-1000 DEG C.The present invention is adopted
Two step reduction method, i.e., first rise to low-temperature reduction temperature from room temperature, be raised again to height at a temperature of low-temperature reduction after held for some time
Warm reduction temperature held for some time, insulation terminate rear furnace cooling to 500 DEG C and anneal, then are pushed into water-cooled area and are cooled to room
Temperature, obtains reduced powder after crushing and screening.Wherein low-temperature reduction temperature is 550-750 DEG C, and temperature retention time is 0.5-2h；High temperature reduction
The temperature time is 1-2h.It is preferred that low-temperature reduction temperature is 600-700 DEG C, temperature retention time is 0.5-1h；More preferably 650 DEG C,
Insulation 45min.High temperature reduction temperature is preferred 930-980 DEG C, is incubated 1.5-2h, more preferably 970 DEG C, is incubated 2h.Reduction process
Reducing atmosphere is H2Atmosphere, gas flow 2L/min, not higher than -40 DEG C of dew point.
During actual intensification, the heating rate for rising to low-temperature reduction temperature from room temperature is 4-15 DEG C/min；From low-temperature reduction temperature
It is 4-20 DEG C/min that degree is raised to the heating rate of high temperature reduction temperature.Preferably, the intensification of low-temperature reduction temperature is risen to from room temperature
Speed is 5 DEG C/min；The heating rate that high temperature reduction temperature is raised to from low-temperature reduction temperature is 5 DEG C/min.
The present invention and its effect are described in further detail with reference to comparative example.
When specifically carrying out contrast test, water atomization low-alloy fecula of the manganese content for 2.5wt.% is chosen, four groups of design is different
Reducing process is analyzed, and its heating schedule is respectively：A1-5 DEG C/min rises to 970 DEG C, is incubated 2h；A2—5℃/min
650 DEG C are risen to, 2h is incubated；A3-5 DEG C/min rises to 650 DEG C, and after insulation 45min, then 5 DEG C/min rises to 970 DEG C, is incubated 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, is incubated 2h.Each group is tested all in H2In atmosphere
Reduced, -35 DEG C of dew point of atmosphere, gas flow 2L/min.Insulation terminates rear furnace cooling to 500 DEG C, then is pushed into water-cooled area
It is cooled to room temperature.
Jing after different process reduction, the essential element content of powder as shown in table 1, is given birth to without the Fe-2.5Mn alloys of reduction
Powder oxygen content 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 is reduced to
0.36%。
The constituent content of 1 Fe-2.5Mn fecula of table powder Jing 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, typically require that powder total oxygen content will be less than 0.2%, by table 1
It can be seen that employing A1 techniques are directly warming up to 970 DEG C of reduction Fe-2.5Mn to be difficult to reach technical requirements.Using A2 techniques, at 650 DEG C
Insulation reductase 12 h, as reduction temperature is low, can only reduce part iron and manganese oxides, and powder total oxygen content is up to 0.49%, it more difficult to reach
To technical requirements.Using A3, A4 technique, insulation reduction, can effectively reduce the total oxygen content of powder in two stages.Particularly A3
Technique, after 650 DEG C of insulation reduction 45min, then rises to 970 DEG C of insulation reductase 12 h, be reduced to can powder total oxygen content
0.16%, requirement of the technical specification to oxygen content can be met.In A4 techniques, by 650 DEG C of holding times to 2h, powder
Total oxygen content have rising again, reach 0.26%.Therefore, technique A3 can prepare guarantee manganese content level do not reduce under the premise of oxygen
The lower water atomization comminuted steel shot of content.
Finally illustrate, above example is only unrestricted to illustrate technical scheme, although with reference to compared with
Good embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to the skill of the present invention
Art scheme is modified or equivalent, and without deviating from the objective and scope of technical solution of the present invention, which all should be covered at this
In the middle of the right of invention.
Claims (4)
1. a kind of hypoxia manganese containing water is atomized the reducing process of comminuted steel shot, water atomization FeMn fecula is carried out also using high temperature reduction method
Original, high temperature reduction temperature are 900-1000 DEG C, it is characterised in that：Using two step reducing process, first low-temperature reduction is risen to from room temperature
Temperature, is raised again to high temperature reduction temperature held for some time at a temperature of low-temperature reduction after held for some time, insulation terminates
Furnace cooling is to less than 500 DEG C afterwards, then is pushed into water-cooled area and is cooled to room temperature；Wherein low-temperature reduction temperature is 550-750 DEG C, insulation
Time is 0.5-2h；The high temperature reduction temperature time is 1-2h.
2. hypoxia manganese containing water as claimed in claim 1 is atomized the reducing process of comminuted steel shot, it is characterised in that：Low temperature is risen to from room temperature
The heating rate of reduction temperature is 4-15 DEG C/min；The heating rate that high temperature reduction temperature is raised to from low-temperature reduction temperature is 4-20
℃/min。
3. hypoxia manganese containing water as claimed in claim 1 is atomized the reducing process of comminuted steel shot, it is characterised in that：Reducing atmosphere is H2Gas
Atmosphere, not higher than -40 DEG C of dew point.
4. hypoxia manganese containing water as claimed in claim 1 is atomized the reducing process of comminuted steel shot, it is characterised in that：Preferred low-temperature reduction
Temperature is 650 DEG C, is incubated 45min；High temperature reduction temperature is 970 DEG C, is incubated 1h.
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| 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 |
| 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 |
| CN106694871B (en) * | 2017-02-28 | 2018-06-19 | 四川理工学院 | Improve the oppressive method of powder containing manganese steel |
| 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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| 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 |
| CN1260841A (en) * | 1997-06-17 | 2000-07-19 | 赫加奈斯公司 | Stainless steel powder |
| CN1288402A (en) * | 1998-01-21 | 2001-03-21 | 赫加奈斯公司 | Steel powder for the prepn. of sintered products |
| CN1410208A (en) * | 2002-11-25 | 2003-04-16 | 莱芜钢铁集团粉末冶金有限公司 | Manufacturing method of alloy steel powder by spraying etc. |
| CN102101174A (en) * | 2009-12-16 | 2011-06-22 | 鞍钢重型机械有限责任公司 | Water atomization diffusion alloy powder and preparation method thereof |
| CN104858444A (en) * | 2015-06-11 | 2015-08-26 | 四川理工学院 | Hypoxic manganese-containing water atomized steel powder reduction process |
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2015
- 2015-06-11 CN CN201510318414.3A patent/CN104858444B/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1260841A (en) * | 1997-06-17 | 2000-07-19 | 赫加奈斯公司 | Stainless steel powder |
| CN1288402A (en) * | 1998-01-21 | 2001-03-21 | 赫加奈斯公司 | Steel powder for the prepn. of sintered products |
| CN1410208A (en) * | 2002-11-25 | 2003-04-16 | 莱芜钢铁集团粉末冶金有限公司 | Manufacturing method of alloy steel powder by spraying etc. |
| CN102101174A (en) * | 2009-12-16 | 2011-06-22 | 鞍钢重型机械有限责任公司 | Water atomization diffusion alloy powder and preparation method thereof |
| CN104858444A (en) * | 2015-06-11 | 2015-08-26 | 四川理工学院 | Hypoxic manganese-containing water atomized steel powder reduction process |
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