CN104630602B - Method for preparing dispersion-strengthened iron-based material by adopting ultrasonic dispersion method - Google Patents
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Abstract
The invention relates to a method for preparing a dispersion-strengthened iron-based material by adopting an ultrasonic dispersion method, belonging to the technical field of powder metallurgy. The method disclosed by the invention comprises the following steps of: putting a certain amount of nanometer oxide powder in alcoholic solution, uniformly dispersing by adopting ultrasonic wave, then, adding iron powder so that the upper surface of the iron powder achieves the height of the liquid level and is parallel to the liquid level, drying in vacuum by putting in a vacuum drying oven to obtain powder with uniformly dispersed nanometer oxide, pressing and forming the powder, sintering at high temperature in vacuum, hot rolling or hot forging so as to obtain a blocky material with uniformly dispersed oxide. By utilizing the simple and convenient ultrasonic dispersion method, nanometer oxide particles in the alcoholic solution are effectively depolymerised and uniformly dispersed, and adsorbed and precipitated on the surface of iron powder in the drying process, so that a uniform mixture is formed; and the method is simple to operate and good in oxide dispersion effect and is applied to large-scale industrial application.
Description
Technical field
The present invention relates to a kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron, belong to powder metallurgy
Technical field.
Background technology
Oxide dispersion intensifying is intensity and the highly effective means of croop property, the mechanical alloy improving metal material
Changing (MA) is the main method preparing Oxide Dispersion Strengthened Materials Made, but this method production efficiency is low, production cost is high, easily dirt
Dye.
For MA method produced problem, have been developed that a series of side preparing Oxide Dispersion Strengthened Materials Made at present
Method.Chinese patent CN1664145A, discloses a kind of chemistry soaking method and prepares the side of oxide dispersion strengthening ferrite alloy
Method, uses chemistry soaking method Y (NO3)3·6H2O solution impregnation pre-alloyed powder, through being dried, hydrogen atmosphere protection heating makes
Be decomposed into Y2O3, thus obtain Y2O3Dispersion strengthening ferrite type alloy powder, then carries out hot densification and prepares block material
Material.Chinese patent CN101823154A, discloses a kind of method using soaking method to prepare oxide dispersion strengthened iron powder, it is provided that
A kind of comprehensively utilize chemistry infiltration and method that high-energy ball milling machinery alloying realizes oxide dispersion strengthened iron powder.China is specially
Profit CN201110154483.7, discloses the preparation side of a kind of nano yttrium oxide dispersed particle-strengthened Alfer powdered steel
Method, is first added to the water ethylenediaminetetraacetic acid and chromic nitrate, stirs at least 12h at 50～60 DEG C, obtains mixed liquor, then to mixed
Close and liquid add citric acid, ferric nitrate, ammonium paratungstate, Yttrium trinitrate and butyl titanate, and at 60～70 DEG C, stir at least 3h,
Obtain colloidal sol；Then, in colloidal sol, first add Polyethylene Glycol, and stir to forming gel at 70～80 DEG C；Finally, the most successively will
Gel is placed at 100～120 DEG C and is dried at least 12h, roasting 4～5h at 300～600 DEG C, obtains oxidation of precursor thing powder, then will
It is placed in reducing atmosphere, calcines at least 3h at 1100～1300 DEG C, prepares the dispersed particle-strengthened ferrite of nano yttrium oxide
Alloy steel powder.
These methods reduce the shortcoming that mechanical alloying is easily polluted to a certain extent, but need to control chemical reaction,
Complex process, operation inconvenience.Meanwhile, the cost of material of chemical powdering method, process costs are high, use a large amount of chemical reagent to draw
Enter impurities left and pollution.
Ultrasonic disperse technology is generally used for dispersion and the homogenization of nano-particle in colloidal dispersion.Nano-oxide particles
It is easily formed colloid in a liquid, and micron-sized metallic powder granule is bigger, it is impossible to form colloid in the solution.Directly utilize super
During metal dust in sound dispersed nano-oxide particles colloid, owing to metal powder granulates exists the difference of granule size
Not, when metal dust adds ultrasound wave scattered nano-oxide particles colloid solution, oarse-grained metal powder is known from experience not
Disconnected absorption nano-oxide particles, causes nano-oxide particles situation pockety occur.The bulky grain that early stage adds
Metal base powder can absorb nano-oxide particles in a large number, and the iron powder bulky grain then entered then only can adsorb remaining to be received on a small quantity
Rice oxide particle, further increases the inhomogeneities of nano-oxide particles distribution.Therefore, ultrasonic uniform point is directly utilized
Dispersed metallic powder and nano-oxide particles also make nano-oxide particles uniformly be attached to have difficulties on metal-powder.
Summary of the invention
The present invention is directed to existing machinery alloying and chemical method prepare oxide dispersion intensifying iron exist easily pollute,
The problems such as control process complexity, oxide easily reunion, it is provided that a kind of employing ultrasonic dispersion prepares dispersion-strengtherning iron
Method.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, comprises the following steps:
Being put into by nano-oxide powder in alcohol liquid, ultrasonic disperse is uniform, after obtaining suspension, in ultrasonic disperse condition
Under, iron-based powder is progressively sent into suspension from the bottom of suspension, until iron-based powder is parallel with liquid level；Then it is dried
To mixed-powder；Finally, mixed-powder is compressing, sintering obtains iron.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, described nano-oxide powder
End is TiO2Or Y2O3；Its granularity is less than or equal to 50nm.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, in described suspension, receives
Rice oxide particle concentration is 17g/L～73g/L；It is preferably 17-50g/L, more preferably 17.5-45g/L.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, it is super that ultrasonic disperse uses
Frequency of sound wave is 20-40kHz.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, the grain of described iron-based powder
Degree, less than or equal to 150 μm, is preferably less than equal to 75 μm.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, described iron-based powder with receive
The mass ratio of rice oxide powder is 99.7:0.3～99:1.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, described alcohol liquid is selected from anhydrous
One in the liquid alcohol such as ethanol, absolute methanol, anhydrous propanol.In order to prevent iron powder surface oxidation, it is beneficial to be dried, reclaim simultaneously
Recycling, the present invention selects conventional anhydrous alcohol solution.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, suspension is adding iron-based
Before powder, sonic oscillation 15-25min, make nano-oxide powder be uniformly dispersed.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, described iron-based powder is from outstanding
The bottom of turbid liquid is successively sent in suspension, until iron-based powder is parallel with liquid level.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, is adding iron-based powder
During, use the synergism with ultrasound wave that successively paves, it is ensured that the nano-oxide in liquid will not be due to ferrous powder granules
Difference in size and occur reunite or flocculation.
The present invention is during powder feeding, it should keep frequency and the power of ultrasound wave so that the acoustic density of ultrasound wave is produced
Raw sufficient cavitation effect, to reach optimal dispersion effect.
The present invention is during powder feeding, and the temperature of suspension is room temperature.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, has added at iron-based powder
After Biing, keep supersonic oscillations 5-10min, make iron powder be dispersed in nano-oxide particles suspension, the most gradually
Reduce supersonic frequency and power so that the cavitation of ultrasound wave gradually reduces, and particulate interspaces is gradually reduced, it is to avoid due to gravity
The phenomenons such as the absorption that cause of effect such as difference are uneven, it is achieved uniform settlement adsorbs.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, described baking temperature is room
Temperature～80 DEG C.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, described compressing pressure
Power is 550-650MPa.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, during described sintering, controls
Vacuum 10-1-10-2Pa, temperature 1050-1200 DEG C, time 3-5h.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron of the present invention, gained iron is through warm
Roll and/or forge hot, obtain finished product；The temperature of described hot rolling and/or forge hot is 850-950 DEG C.
Advantages of the present invention and good effect:
Iron-based powder, under ultrasound condition, is successively sent into suspension by the present invention from the bottom of suspension, until iron-based
Powder is parallel with liquid level；Make iron-based powder enter suspension time only can adsorb iron-based powder position aspect in and on
The nano-oxide of portion's close position, it is achieved iron-based powder successively adsorbs nano-oxide, makes nano-oxide at iron-based powder
It is uniformly distributed；It addition, under the effect of ultrasonic energy, the nano-oxide less with iron-based powder adhesion, it is possible to depart from
The absorption of iron-based powder, reenters suspension, is adsorbed by the iron-based powder of follow-up entrance, is effectively improved nano-oxide distribution
Uniformity；On the other hand, ultrasonic vibration energy can effectively stop the reunion between nano-oxide or flocculation, it is ensured that nanometer
The uniformity that oxide is distributed in iron-based powder.
When the present invention adds iron-based powder, keeping the frequency of former ultrasound wave and power at 20-40Hz, preferably 30Hz is left
Right so that the acoustic density of ultrasound wave produces sufficient cavitation effect, reaches optimal dispersion effect.Meanwhile, suitable ultrasonic
Frequency can also promote the nano-oxide will reunited or flocculate to obtain dispersed, and this has further ensured that nano oxidized
The dispersion effect of thing.
When the present invention adds iron-based powder, suspension temperature is room temperature, it is not necessary to control especially.Iron powder add complete it
After, keep supersonic oscillations 5-10min, make nano-oxide particles and iron powder fully dispersed, be gradually lowered supersonic frequency afterwards,
The cavitation making ultrasound wave slowly reduces, and particulate interspaces is gradually reduced, thus avoids owing to the effects such as gravitational difference cause
The phenomenons such as absorption is uneven, it is achieved uniform settlement adsorbs.
Present invention achieves nano-oxide particles to mix, for obtaining high-quality disperse iron-based material with the uniform of iron-based powder
Material provides essential condition.
The present invention solves the contingent agglomeration traits of disperse oxide, it is achieved the disperse of nano-oxide uniformly divides
Cloth；Overcome mechanical alloying and prepare the shortcomings such as dispersed oxide easily pollutes, control process is complicated with chemical method.
In a word, the present invention uses and first disperses, and decomposite technology path i.e. utilizes ultrasonic disperse technology by nano-oxide
Even particulate dispersion, in room temperature liquid, adds iron-based powder and is allowed to mix, be finally dried, make nano-oxide particles adhere to
On iron-based powder；Utilize easy ultrasonic dispersion, it is achieved effective depolymerization of nano-oxide particles in alcoholic solution, uniformly
Dispersion and distribution, by follow-up being dried, compacting, sintering processes obtained the dispersion-strengtherning iron of superior performance.This
Bright preparation technology is simple, and nano-oxide particles disperse is effective, is suitable to large-scale industrial application.
Detailed description of the invention
Embodiment 1:
Preparation 0.5 (wt) %TiO2Dispersion-strengtherning iron, its process is as follows:
(1) under ultrasound condition, granularity is less than or equal to the TiO of 10nm2Material powder (Detitanium-ore-type), adds without ethanol
In solution, sonic oscillation 15min, make TiO2Powder is uniformly dispersed, and obtains the suspended liquid that material powder concentration is 18g/L, super
The frequency of sound wave is 30kHz；
(2) keeping under ultrasound condition, be the iron-based powder less than or equal to 150 μm with funnel by granularity, bottom vessel
At the uniform velocity handling powder feeding, in successively tiling to prepared suspended liquid, until iron-based powder is parallel with liquid level, obtains mixture；
During powder feeding, keep frequency and the power of former ultrasound wave, make the acoustic density of ultrasound wave produce sufficient cavitation effect,
Reaching optimal dispersion effect, solution temperature is maintained at room temperature.After iron powder addition is complete, keep supersonic oscillations 8min,
Make iron powder be dispersed in nano-oxide particles alcohol suspending liquid, be then gradually lowered supersonic frequency and power, until stopping
The most ultrasonic；
(3) to gained mixture after room temperature, normal pressure are dried process, dispersion-strengtherning iron-based is obtained through pressed compact, sintering
Material.During pressed compact, control pressure is 550MPa；The condition of sintering is: vacuum 10-1-10-2Pa, temperature 1050 DEG C, the time
3.5h。
(4) sintered body is carried out forge hot, forging temperature 850 DEG C, it is thus achieved that nano-TiO2Dispersion strengthened iron.
Embodiment 2:
Preparation 1% (wt) Y2O3Dispersion strengthened iron, its process is:
(1) configuration concentration is the Y of 36g/L2O3Ethanol solution, wherein Y2O3Granularity is less than or equal to 30nm, molten by configured
Liquid utilizes ultrasonoscope sonic oscillation 15min to make nanometer Y2O3It is uniformly dispersed；The frequency of ultrasound wave is 40kHz；
(2) under keeping ultrasound condition, with funnel, granularity is less than or equal to the iron-based powder of 75 μm, bottom vessel at the uniform velocity
Successively tiling is in the most prepared suspended liquid, until iron-based powder upper surface reaches liquid level parallel with liquid level；Keep
Supersonic oscillations 10min；Then supersonic frequency and power it are gradually lowered, until stopping ultrasonic；
(3) mixture prepared by (2nd) step being inserted vacuum drying oven to be dried, baking temperature is 80 DEG C, drying time
30min；
(4) dried mixed-powder is inserted mould, use 600MPa pressure compressing, prepare nano oxidized
Thing equally distributed pressed compact body；
(5) pressed compact is inserted vacuum sintering furnace and carries out vacuum-sintering, 1200 DEG C of sintering 1h, prepare nano-oxide equal
The sintered body of even distribution；
(6) sintered blank carrying out hot rolling shaping, hot-rolled temperature 950 DEG C, forging densification obtains nanometer Y2O3Dispersion strengthened iron.
Embodiment 3:
Preparation 0.5 (wt) %Y2O3Dispersion strengthened iron, its process is:
(1) under ultrasound condition, granularity is less than or equal to the Y of-10nm2O3Material powder, adds in anhydrous alcohol liquid,
Sonic oscillation 15min, makes Y2O3Powder is uniformly dispersed, and obtains the suspended liquid that material powder concentration is 18g/L, the frequency of ultrasound wave
Rate is 30kHz；
(2) keeping under ultrasound condition, be the iron-based powder less than or equal to 75 μm with funnel by granularity, even bottom vessel
Speed successively tiling is in the most prepared suspended liquid, until iron-based powder upper surface reaches liquid level parallel with liquid level,
To mixture；During powder feeding, it should keep frequency and the power of former ultrasound wave so that the acoustic density of ultrasound wave produces
Sufficiently cavitation effect, reaches optimal dispersion effect, and solution temperature is maintained at room temperature.After iron powder addition is complete, keep
Supersonic oscillations 5min, make iron powder be dispersed in nano-oxide particles alcohol suspending liquid, are then gradually lowered supersonic frequency
Rate and power so that the cavitation of ultrasound wave gradually reduces, until stopping ultrasonic.
(3) to gained mixture after room temperature, normal pressure are dried process, dispersion-strengtherning iron-based is obtained through pressed compact, sintering
Material.During pressed compact, control pressure is 600MPa；The condition of sintering is: vacuum 10-1-10-2Pa, temperature 1050 DEG C.
(4) sintered blank is carried out hot forging forming, forging temperature 900 DEG C, it is thus achieved that nanometer Y2O3Dispersion strengthened iron.
Claims (10)
1. one kind uses the method that ultrasonic dispersion prepares dispersion-strengtherning iron, it is characterised in that: by nano-oxide
Powder is put in alcohol liquid, and ultrasonic disperse is uniform, after obtaining suspension, under the conditions of ultrasonic disperse, by iron-based powder from suspension
Bottom successively send in suspension, until iron-based powder is parallel with liquid level；Then uniform mixed-powder it is dried to obtain, then will be mixed
Close powder pressing, sintering, obtain iron.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron the most according to claim 1, it is special
Levy and be: the ultrasonic frequency that ultrasonic disperse uses is 20-40kHz.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron the most according to claim 1, it is special
Levy and be: described nano-oxide powder is TiO2Or Y2O3；Its granularity is less than or equal to 50nm.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron the most according to claim 1, it is special
Levying and be: in described suspension, nano-oxide particles concentration is 17g/L～73g/L.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron the most according to claim 1, it is special
Levy and be: the granularity of described iron-based powder is less than or equal to 150 μm；Described iron-based powder with the mass ratio of nano-oxide powder is
99.7:0.3～99:1.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron the most according to claim 1, it is special
Levy and be: described alcohol liquid one in dehydrated alcohol, absolute methanol, anhydrous propanol.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron the most according to claim 1, it is special
Levy and be: the temperature of suspension is room temperature.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron the most according to claim 1, it is special
Levy and be: after iron-based powder addition is complete, keep supersonic oscillations 5-10min.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron the most according to claim 1, it is special
Levy and be:
Described baking temperature is room temperature～80 DEG C；
Described compressing pressure is 550-650MPa；
During described sintering, control vacuum 10-1-10-2Pa, temperature 1050-1200 DEG C, time 3-5h.
A kind of method using ultrasonic dispersion to prepare dispersion-strengtherning iron the most according to claim 1, it is special
Levy and be: gained iron is hot rolled or forge hot, obtains finished product；The temperature of described hot rolling or forge hot is 850-950 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP3868491A1 (en) * | 2020-02-21 | 2021-08-25 | General Electric Company | Methods of manufacturing dispersion strengthened materials |
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| CN115446302B (en) * | 2022-08-31 | 2024-04-19 | 鞍钢股份有限公司 | Iron-based intermediate with uniformly dispersed nano particles and preparation and use methods thereof |
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| CN102994884A (en) * | 2012-12-03 | 2013-03-27 | 东北大学 | Efficient preparation method for nanostructure oxide dispersion strengthening steel |
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|---|---|---|---|---|
| CN1664145A (en) * | 2005-04-04 | 2005-09-07 | 北京科技大学 | Process for producing oxide dispersion strengthening ferrite type alloy by using chemical dipping method |
| CN101476063A (en) * | 2008-12-22 | 2009-07-08 | 沈阳工业大学 | Nano composite nickel substitute alloy and manufacturing process thereof |
| CN102994884A (en) * | 2012-12-03 | 2013-03-27 | 东北大学 | Efficient preparation method for nanostructure oxide dispersion strengthening steel |
| CN103233182A (en) * | 2013-06-07 | 2013-08-07 | 北京科技大学 | Forming method for nanometer beta' phase element and nanometer oxide composite reinforced Fe-based ODS alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3868491A1 (en) * | 2020-02-21 | 2021-08-25 | General Electric Company | Methods of manufacturing dispersion strengthened materials |
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