CN106735307B - The water atomization comminuted steel shot oxygen content of prealloy containing manganese regulates and controls method - Google Patents
The water atomization comminuted steel shot oxygen content of prealloy containing manganese regulates and controls method Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
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- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a kind of water atomization prealloy containing manganese comminuted steel shot oxygen content regulate and control method, 1)Water atomization is used to prepare manganese content as 1.0% or more water atomization fecula;2)Deployed pickling solution is added in the reactor, adds step 1)The fecula of preparation carries out pickling and is finally washed with washing off the oxidation film on water atomization fecula surface, and hydrogen ion content and the molar ratio of the total oxygen element content of fecula are slightly larger than 2 in pickle:1;Pickling time 10 30 minutes;Filter to obtain fecula;3)Dry and remove the moisture in fecula;4)Fecula after drying is 900 DEG C 1000 DEG C in maximum temperature, and dew point is less than 40 DEG C of H2High temperature reduction processing, 1 2h of high temperature reduction time are carried out in atmosphere.The present invention can control pre-alloyed powder oxygen content≤1500ppm that Mn contents are 1.0 5.0%.And prior art pre-alloyed powder oxygen content is usually 0.5 1.5%.
Description
Technical field
The present invention relates to the preparations of the comminuted steel shot of prealloy containing manganese, refer specifically to the water atomization comminuted steel shot oxygen content of prealloy containing manganese regulation and control side
Method belongs to powder metallurgical technology.
Background technology
China's iron-base powder metallurgical product development space is wide, and by taking automobile industry as an example, China produces automobile more than 2,000 ten thousand per year
, but since technical merit restricts, the iron-based powder metallurgy parts amount used on each automobile of China is and Europe, beautiful less than 5Kg
The iron-based powder metallurgy parts amount used on each automobile of Guo Deng developed countries has reached 14-19.5Kg.If each automobile of China increases
Add 9Kg iron-based powder metallurgy parts, annual near reduce adds the demand of 180,000 tons of steel powders and ferrous based powder metallurgical parts.
Therefore, China's steel powder is improved to the preparation level of iron-based powder metallurgy parts for China's ferrous based powder metallurgical and related production
Industry development is of great significance.
Prior powder metallurgy iron-based material generally uses Ni, Cu etc. to be used as intensified element, since Ni may make human body
At harm, Cu recyclings are difficult, and nonferrous metal price is high, and researcher is promoted to seek to be suitable for sintered steel
New alloy element.Mn elements rich reserves on earth, it is cheap, it is best to the reinforcing effect of steel, as alloying element
It is successfully used for forge steel for many years, and the densification of iron-based material containing Mn can flexibly select room temperature sintering, high temperature sintering or sinter-hardened
Technology, therefore Mn is introduced into the hot spot for becoming research in iron-based powder as alloying element.
It is that manganese element oxytropism is strong to hinder the principal element of this kind of Materials, is prepared in powder easy with manganese in sintering process
Oxidation, it is more difficult to restore.There are three types of modes as alloying element introducing for manganese:Element powders method, master alloy method and atomization.With element
Its oxidation of powder type addition manganese is most apparent;To inhibit manganese in the oxidation of powder metallurgy process, can be used by manganese and iron, chromium, molybdenum,
The mode that the elements melting such as carbon forms master alloy introduces manganese, makes manganese from oxidation by forming complicated carbide, but this method exists
Cost, suppression performance and product size control aspect Shortcomings;Water atomization is a kind of low cost system of the powder containing manganese alloy steel
Alloying, activity reduce in water atomization fecula standby technology, iron and manganese, inhibit manganese to a certain degree in the subsequent process
Oxidation and distillation.
During water atomization, high-temperature molten steel forms molten drop under the impact of water, and high temperature drop contacts generation with water
Vigorous oxidation is reacted, and layer oxide film is formed on molten drop surface.Research shows that oxidation film mainly contains ferriferous oxide FexOy、
Ferro manganese composite oxides FeMn2O4And the oxides such as MnO.Wherein ferriferous oxide and ferro manganese composite oxides are respectively at 400-700 DEG C
It can be by H with 700 DEG C or more2It is restored with CO, and MnO is difficult to by H2Reduction, need in 1200-1300 DEG C of ability completely by C also
Original, oxygen content in power is still very high after reduction.Therefore the oxygen content in control powder raw material and agglomerated material is always low containing Mn
The focus of alloy powder metallurgy investigation of materials and exploitation.
Kawasaki, Japan Zhi Gang companies are directed to the problem that oxygen content is high in atomized powder containing manganese, develop water atomization-vacuum also
Former technology.But vacuum reduction is very high to equipment requirement, and cannot achieve large-scale continuous production.Hoeganaes is then developed
Water atomization-high temperature reduction technology, which employs at least in 1120 DEG C or more of reduced anneal technique.However at 1120 DEG C or more
High annealing powder agglomates will be made serious, greatly increase the broken difficulty of subsequent technique, force broken also easily powder to be made to be formed
Processing hardening reduces the compressibility energy of powder.The reduction system for being 970 DEG C for China's water-atomized iron powder highest reduction temperature
System, Sichuan University of Science & Engineering and Central South University's joint development two benches reduction techniques first restore easy reduction in the low-temperature reduction stage
Ferriferous oxide, with reduce hot stage oxidation shift and regulation and control high temperature reducing atmospheres dew point, the oxygen of powder can also be contained
Amount be reduced to 0.2% hereinafter, but 970 DEG C of reduction temperature it is poor to the reduction effect of Mn oxide, there is more oxygen island on surface.
E. Hryha et al. carries out the surface composition of the alloy steel powder by spraying etc. of the Hoeganaes four kinds of manganese contents provided
Research finds that the more oxygen island being made of Mn oxide is contained on the powder surface after reduction, and with the increase of manganese content, oxygen island
Volume is bigger, and quantity is more, and the ratio for accounting for powder surface area is also bigger.Oxygen island is difficult to restore in the subsequent sintering process, sintering
Mn oxide is still present on the neck interface that particle is formed with particle afterwards, hinders the connection between particle.The smelting of end containing manganese powder
Golden steel construction piece will have good sinterability energy, just necessarily require the coverage rate on powder Surface Oxygen island to be less than 10%, total oxygen contains
Amount is less than 0.2%.
Water atomization pulverization and the temperature of reduced anneal are higher, and manganese can occur to aoxidize transfer reaction, and manganese element is caused to exist
Powder surface aggregation.The research of Central South University dragon Anping, Li Songlin et al. and E. Hryha et al. can confirm this point.Also
The surface layer manganese element content of powder is far above the inside of powder after original, and depth is up to 10 nm.Manganese is unfavorable in the concentration of powder face
Inhibit the oxidation of manganese in subsequent technique, and further improve the surface hardness of powder, reduces the compression performance of powder.
Compressibility is one of most important processing performance of steel powder product, the conditions such as pressing pressure, mold tooling not
In the case of change, powder compressibility directly decides the density and its mechanical property of part.Manganese element has steel strong well
Change effect, oxygen content height can also increase powder hardness, manganese and oxygen in powder surface aggregation, further improve powder face
Hardness causes the comminuted steel shot processability of prealloy containing Mn poor.Such as Fe-Mn powder containing 1.5%Mn and 2.0%Mn is suppressed under 600MPa
Powder of the density ratio without Mn reduces 0.15g cm respectively-3With 0.2g cm-3More than, part sintering character or ruler will necessarily be influenced
Very little, this is also one of the reason that Mn contents are not high in the low alloyed steel powder that each major company produces at present.External powdered alloy steel product
Middle Mn highests content is less than 1% mostly, and the country is often below 0.5%, and alloying element content is generally in low-alloy steel powder
1.5-5.0%, for reducing cost angle, Mn contents also have certain rising space.Therefore processability difference is to hinder to contain Mn
Another key factor of prealloy comminuted steel shot development.
Invention content
For deficiencies of the prior art, the object of the present invention is to provide a kind of water atomization prealloy containing manganese comminuted steel shots
Oxygen content regulates and controls method, and this method can substantially reduce the oxygen content in the pre-alloyed powder containing manganese of water atomization preparation.
The technical proposal of the invention is realized in this way:
The water atomization comminuted steel shot oxygen content of prealloy containing manganese regulates and controls method, and steps are as follows,
1)It is prepared by fecula
Water atomization is used to prepare manganese content as 1.0% or more water atomization fecula;
2)Pickling
In the reactor with stirring, deployed pickling solution is added, adds step 1)The fecula of preparation carries out
Pickling is finally washed with washing off the oxidation film on water atomization fecula surface, is stirred continuously in pickling and water-washing process, speed of agitator
50-100 revs/min, to improve pickling and water washing effect;Mole of hydrogen ion content and the total oxygen element content of fecula in pickle
Than being slightly larger than 2:1;Pickling time 10-30 minutes;Filter to obtain fecula;
3)It is dry
It is dry at a temperature of 100 DEG C -200 DEG C, remove the moisture in fecula;
4)High temperature reduction
By step 3)Fecula after drying is 900 DEG C -1000 DEG C in maximum temperature, and dew point is less than -40 DEG C of H2In atmosphere
Carry out high temperature reduction processing, high temperature reduction time 1-2h.
Further, also include the following steps successively after high temperature reduction,
5)Displacement plating
In the reactor with stirring, deployed ferrous salt solution is added, adds the alloyed powder after high temperature reduction,
It is reacted into line replacement, replaces and be stirred continuously in reaction process, 50-100 revs/min of speed of agitator is set using the manganese in alloyed powder
The ferrous ion in ferrous salt solution is changed, to form porous plating iron layer and loose demanganize layer on powder surface, water after replacement completion
It washes;It is dry at a temperature of 100 DEG C -200 DEG C after washing, to remove moisture;Ferrous salt is frerrous chloride or ferrous sulfate, reaction
Time 1-2 hour;
6)Low-temperature reduction is annealed
To step 5)For powder after displacement at 600-800 DEG C, dew point is less than -40 DEG C of H2Low-temperature reduction is carried out in atmosphere to move back
Fire processing, processing time 1-2h.
Compared with prior art, the present invention has the advantages that:
1, the present invention regulates and controls the oxygen content of alloyed powder using pickling in such a way that reduction is combined, and is easily removed using pickling
The characteristic of oxidation on metal surface object first passes through pickling and washes off water atomization fecula oxidation film, the method for restoring remaining oxygen in powder,
To regulate and control oxygen content in power.By acid cleaning process, the present invention can control the pre-alloyed powder oxygen that Mn contents are 1.0-5.0%
Content≤1500ppm.And prior art pre-alloyed powder oxygen content is usually 0.5-1.5%.
2, the present invention is formed porous using the ferrous ion in the manganese displacement ferrous salt solution in alloyed powder on powder surface
Iron layer and loose demanganize layer are plated, alloy powder surface layer microhardness is reduced, regulates and controls powder compacting performance.By replacing depositing process,
The present invention can control pre-alloyed powder surface layer microhardness≤80 HV that Mn contents are 1.0-5.0%, compressibility >=7.1g
cm-3(600MPa is suppressed).
Description of the drawings
Fig. 1-present invention process flow chart.
Specific implementation mode
Technical scheme of the present invention is described in detail below in conjunction with the accompanying drawings.
Water atomization prealloy containing manganese comminuted steel shot oxygen content regulation and control method of the present invention is as follows, and Fig. 1 is shown in technological process.
1)It is prepared by fecula
Design alloying element formula, a series of water atomization fecula for using water atomization to prepare manganese content as 1.0-5.0%.
Water atomization fecula, that is, water atomization the comminuted steel shot of prealloy containing manganese, final products are comminuted steel shots, also need to restore after water atomization, before reduction, referred to as
For fecula.
2)Pickling
In the reactor with stirring and temperature regulating device, deployed pickling solution is added, adds step 1)It prepares
Fecula carry out pickling finally washed with washing off the oxidation film on water atomization fecula surface;Pickle can be hydrochloric acid, sulfuric acid, ice
The weak solution of the conventional acids such as acetic acid, dosage is depending on oxygen content in fecula, and oxygen content is 2% or so in general fecula, and acid can be with
Slightly excessive, by taking hydrochloric acid as an example, one ton of fecula can add the dilute hydrochloric acid of one ton of a concentration of 4.4%-6% to carry out pickling, can also add
The dilute hydrochloric acid of two tons of a concentration of 2.2%-3% carries out pickling, not strict regulations, only requires solution hydrogen ion content and the total oxygen member of fecula
The molar ratio of cellulose content is slightly larger than 2:1;Pickling sustained release agent is general pickling sustained release agent, and dosage can be according to the use of pickling used
Illustrate to be matched.Reaction temperature room temperature, reaction time 10-30 minute.It is dry at a temperature of 100 DEG C -200 DEG C after washing, it removes
Remove the moisture in fecula;
3)High temperature reduction
By step 2)Fecula after pickling is at 900-1000 DEG C, the H that dew point is -40 DEG C2It is carried out at high temperature reduction in atmosphere
Reason, high temperature reduction time 1-2h.
The oxygen content in comminuted steel shot after restoring is measured using TC600 nitrogen/oxygen instrument, the results showed that, the present invention can be controlled effectively
The oxygen content of pre-alloyed powder containing Mn can make oxygen content≤1500ppm in the comminuted steel shot after reduction.
4)Displacement plating
In the reactor with stirring and temperature regulating device, deployed ferrous salt solution is added, adds high temperature reduction
Alloyed powder afterwards is reacted into line replacement, using the ferrous ion in the manganese displacement ferrous salt solution in alloyed powder, in powder table
Face forms porous plating iron layer and loose demanganize layer, is washed after replacement completion;It is equally done at a temperature of 100 DEG C -200 DEG C after washing
It is dry, to remove moisture;Ferrous salt can be frerrous chloride, also can be ferrous sulfate.By taking ferrous sulfate solution dosage as an example, one
Ton powder containing manganese steel, can add the ferrous sulfate solution of one ton of a concentration of 2%-5% to be impregnated, reaction temperature room temperature, the reaction time
1-2 hours.
5)Low-temperature reduction is annealed
Using the H that at 600-800 DEG C, dew point is -40 DEG C2In atmosphere the technological parameter of reductase 12 h to the powder after displacement into
Row low-temperature reduction makes annealing treatment.
The alloyed powder compacting and sintering character research that the present invention obtains:The reduced powder of finally obtained each ingredient is equipped with
The graphitic carbon of 0.5wt.% is used in combination zinc stearate to carry out outer lubrication, is suppressed under 600MPa pressing pressures using one-way press, pressed
Density processed >=7.1g cm-3。
Embodiment 1:
1)It is prepared by fecula:Water atomization is used to prepare manganese content as 2.7% water atomization fecula.
2)Pickling:The sulfuric acid solution that mass concentration is 2.5% is added in the reactor, adds step 1)The fecula of preparation
It carries out pickling finally to wash to wash off the oxidation film on water atomization fecula surface, pickling and water-washing process are stirred continuously, and stirring turns
68 revs/min of speed;Sulfuric acid solution hydrogen ion content is 2.14 with the total oxygen element content molar ratio of fecula:1;25 DEG C of pickling temperature,
Pickling time 23 minutes.It is dried after washing.
3)High temperature reduction:By fecula at 980 DEG C, H that dew point is -40 DEG C2High temperature reduction processing is carried out in atmosphere, high temperature is also
Former time 1.8h.Oxygen content test shows that oxygen content is 1440ppm in comminuted steel shot after reduction.
4)Displacement plating:The ferrous sulfate solution 200g that mass concentration is 3.5% is added in the reactor, adds high temperature also
Alloyed powder 200g after original is reacted into line replacement, reaction temperature room temperature, 1.8 hours reaction time;It is washed after replacement completion;Washing
After be dried.
5)Low-temperature reduction is annealed:Using the H that at 750 DEG C, dew point is -40 DEG C2The technological parameter of reductase 12 h is opposed in atmosphere
Powder after changing carries out low-temperature reduction annealing.The pressed density of final products is 7.45g cm-3。
Embodiment 2:
1)It is prepared by fecula:Water atomization is used to prepare manganese content as 4.4% water atomization fecula.
2)Pickling:The hydrochloric acid solution that mass concentration is 5% is added in the reactor, adds step 1)The fecula of preparation into
Row pickling is finally washed with washing off the oxidation film on water atomization fecula surface, and pickling and water-washing process are stirred continuously, speed of agitator
60 revs/min;Hydrochloric acid solution hydrogen ion content is 2.1 with the total oxygen element content molar ratio of fecula:1;25 DEG C of pickling temperature, pickling
20 minutes time.It is dried after washing.
3)High temperature reduction:By fecula at 970 DEG C, H that dew point is -40 DEG C2High temperature reduction processing is carried out in atmosphere, high temperature is also
Former time 2h.Oxygen content test shows that oxygen content is 1430ppm in comminuted steel shot after reduction.
4)Displacement plating:The solution of ferrous chloride 150g that mass concentration is 3% is added in the reactor, adds high temperature reduction
Alloyed powder 120g afterwards is reacted into line replacement, reaction temperature room temperature, 1.6 hours reaction time;It is washed after replacement completion;After washing
It is dried.
5)Low-temperature reduction is annealed:Using the H that at 680 DEG C, dew point is -40 DEG C2The technological parameter pair of 1.6h is restored in atmosphere
Powder after displacement carries out low-temperature reduction annealing.The pressed density of final products is 7.38g cm-3。
One, pickling-reduction method regulation and control oxygen content principle illustrates.
Using on acid solution removal steel surface oxide skin and the method for rust be known as pickling, frequently as being electroplated, ward off
The pre-treatment of the techniques such as porcelain, rolling or intermediate treatment are the highly developed effective method of one kind for cleaning metal surface, manganese containing water
Fecula oxygen content is atomized generally between 0.5-1.5%, and most oxidation films for concentrating on powder surface, it is former needed for pickling
Material and fecula loss are seldom, and scientific basis is provided to remove powder surface film oxide using acid wash.The big portion of Mn oxide
Dividing is formed in atomization step, is concentrated mainly on the oxidation film on fecula surface again, and hardly possible reduction is but easy to pickling removal, and
At least be conducive to the control of oxygen content in reduction process at following three aspect:
1)Inhibit oxidation transfer.Pickling can remove fecula surface iron-oxides, inhibit in annealing reduction process manganese element with
The oxidation transfer that ferriferous oxide occurs;
2)Regulate and control furnace reduction dew point of atmosphere.Water atomization fecula generally uses hydrogen reducing, and manganese oxytropism is strong, to being gone back in stove
The dewpoint requirements of Primordial Qi atmosphere are very strict, and current industrial reducing gas dew point can reach requirement.But the oxygen carried in fecula
It can be reacted with hydrogen, so that the dew point of furnace reduction atmosphere is increased rapidly, fecula oxygen content can be greatly lowered in pickling, be conducive to regulate and control
Furnace reduction dew point of atmosphere;
3)Promote Mn oxide reduction.Excessive carbon can generally be added during cast iron melting with the oxygen for reducing molten iron to contain
Amount, sequential reduction annealing temperature is generally greater than 900 DEG C, and more than this temperature, carbon ratio hydrogen has stronger reducing power.If
Ferriferous oxide oxygen content is higher in fecula, and at 800 DEG C preferentially with ferriferous oxide decarburizing reaction can occur for carbon.Pickling can remove life
Most of ferriferous oxide, excessive carbon can remain into higher temperature, promote the carbon thermal reduction of Mn oxide in powder.
Two, displacement method regulation and control processability principle illustrates.
It is reacted using displacement, reduces powder face manganese content, form loose demanganize layer and porous plating iron layer, reduce powder table
Layer microhardness, to improve powder compacting performance.It is surface modified by powder, surface hardness is reduced, is to improve hard
The effective way of alloy powder compression performance, the analysis of causes are as follows:Plastic deformation is the main machine of alloy powder compressing and compacting
System, stress deformation model in analysed for powder pressing process it is found that powder center by the compression in all directions almost
It is impartial, constrains its plastic deformation, and powder face is mainly by the compression perpendicular to powder and powder contact surfaces,
It is that powder accumulates the gap to be formed to be parallel to contact surface direction, does not generate constraint to plastic deformation.Therefore in pressing process, powder
End is big with the surface layer plastic deformation at powder contact, and closer to center, plastic deformation is smaller.Therefore it is hard to reduce powder face
Degree is the effective ways for improving cemented carbide powder compression performance.
The present invention regulates and controls processability using pickling-reduction method regulation and control oxygen content and displacement method, and manganese containing water atomization can be made to close
Golden comminuted steel shot has both performance and price advantage simultaneously.
Traditional water atomization-reduction method prepares manganese containing water atomized alloy powder, and manganese element and oxygen element are in powder surface aggregation, sternly
The compression of damage powder and sintering character again, cause in alloyed powder manganese can addition be less than 1%.The present invention is using pickling dissolving life
The method of powder oxidation film can solve Mn oxide and be difficult to restore the sciences problems of removal;It is formed on powder surface using displacement method
The method of loose demanganize layer and porous plating iron, can solve the technical barrier of powder compacting poor performance.To be expected to prepare manganese content
For the water atomization alloyed powder of 1.5-5%, Mn elements rich reserves on earth are cheap, good to the reinforcing effect of steel.Cause
This has both performance and price advantage simultaneously with traditional water atomization-reducing process ratio, the present invention.
Alloying element content is generally 1.5-5.0% in low-alloy steel powder, and manganese content is higher than 1% low alloyed steel powder at present
Prepared by powder metallurgy material needs additional manganese source powder, and in order to obtain good uniformity and consistency, the prior art preferably solves
Certainly scheme is to use pre-mixed technology.Premix containing manganese is exactly the surface for manganese source powder being adhered to using binder iron powder,
And manganese is unfavorable for inhibiting the oxidation and distillation of manganese in subsequent technique in the concentration on powder surface.And the acid wash that the present invention uses and
Displacement method is simple for process, and consumption of raw materials is few, of low cost, and gained powder has center manganese content high, and surface manganese content is low
Architectural characteristic, which can not only inhibit the oxidation and distillation of manganese in subsequent technique, can with Effective Regulation powder at
Type performance.Only Ji Jia major companies of foreign countries have grasped pre-mixed technology at present, and premix is the 3-4 of China's iron powder price
Times.Therefore compared with premix, the present invention has both performance and price advantage simultaneously.
The above embodiment of the present invention is only example to illustrate the invention, and is not the embodiment party to the present invention
The restriction of formula.For those of ordinary skill in the art, other differences can also be made on the basis of the above description
The variation and variation of form here can not be exhaustive all embodiments.It is every to belong to technical scheme of the present invention institute
Row of the obvious changes or variations amplified out still in protection scope of the present invention.
Claims (2)
1. the water atomization comminuted steel shot oxygen content of prealloy containing manganese regulates and controls method, it is characterised in that:Steps are as follows,
1)It is prepared by fecula
Water atomization is used to prepare manganese content as 1.0% or more water atomization fecula;
2)Pickling
In the reactor with stirring, deployed pickling solution is added, adds step 1)The fecula of preparation carries out pickling,
It to wash off the oxidation film on water atomization fecula surface, finally washes, is stirred continuously in pickling and water-washing process, speed of agitator 50-100
Rev/min, to improve pickling and water washing effect;Hydrogen ion content and the molar ratio of the total oxygen element content of fecula are more than in pickle
2:1;Pickling time 10-30 minutes;Filter to obtain fecula;Pickling solution is the weak solution of hydrochloric acid, sulfuric acid or glacial acetic acid;
3)It is dry
It is dry at a temperature of 100 DEG C -200 DEG C, remove the moisture in fecula;
4)High temperature reduction
By step 3)Fecula after drying is 900 DEG C -1000 DEG C in maximum temperature, and dew point is less than -40 DEG C of H2It is carried out in atmosphere high
Warm reduction treatment, high temperature reduction time 1-2h;
5)Displacement plating
In the reactor with stirring, deployed ferrous salt solution is added, adds the alloyed powder after high temperature reduction, carries out
Displacement reaction, replaces and is stirred continuously in reaction process, 50-100 revs/min of speed of agitator, is replaced using the manganese in alloyed powder sub-
Ferrous ion in iron salt solutions is washed with forming porous plating iron layer and loose demanganize layer on powder surface after replacement completion;Water
It is dry at a temperature of 100 DEG C -200 DEG C after washing, to remove moisture;Ferrous salt is frerrous chloride or ferrous sulfate, reaction time
1-2 hours;
6)Low-temperature reduction is annealed
To step 5)For powder after displacement at 600-800 DEG C, dew point is less than -40 DEG C of H2It is carried out at low-temperature reduction annealing in atmosphere
Reason, processing time 1-2h.
2. water atomization prealloy containing manganese comminuted steel shot oxygen content according to claim 1 regulates and controls method, it is characterised in that:Step 4)
In high temperature reduction, reduction temperature is 970 DEG C, recovery time 2h.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN201710111699.2A CN106735307B (en) | 2017-02-28 | 2017-02-28 | The water atomization comminuted steel shot oxygen content of prealloy containing manganese regulates and controls method |
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CN102990052A (en) * | 2011-09-16 | 2013-03-27 | 于国锋 | Preparation and storage method of active iron powder |
CN103506618A (en) * | 2013-10-15 | 2014-01-15 | 中南大学 | Mn-contained mixture steel powder for powder metallurgy and preparing method |
CN103602920A (en) * | 2013-11-25 | 2014-02-26 | 山东时雨轴承有限公司 | Bearing steel and manufacturing process of wear-resistant bearing |
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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CN102990052A (en) * | 2011-09-16 | 2013-03-27 | 于国锋 | Preparation and storage method of active iron powder |
CN103506618A (en) * | 2013-10-15 | 2014-01-15 | 中南大学 | Mn-contained mixture steel powder for powder metallurgy and preparing method |
CN103602920A (en) * | 2013-11-25 | 2014-02-26 | 山东时雨轴承有限公司 | Bearing steel and manufacturing process of wear-resistant bearing |
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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