CN104630602A - Method for preparing dispersion-strengthened iron-based material by adopting ultrasonic dispersion method - Google Patents
Method for preparing dispersion-strengthened iron-based material by adopting ultrasonic dispersion method Download PDFInfo
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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 adopting ultrasonic dispersion to prepare dispersion-strengthened iron, belong to powder metallurgical technology.
Background technology
Oxide dispersion intensifying is the intensity and the highly effective means of creep property that improve metallic substance, mechanical alloying (MA) is the main method preparing Oxide Dispersion Strengthened Materials Made, but this method production efficiency is low, production cost is high, easily pollute.
For MA method produced problem, develop a series of method preparing Oxide Dispersion Strengthened Materials Made at present.Chinese patent CN1664145A, discloses the method that the chemical soaking method of a kind of use prepares oxide dispersion strengthening ferrite alloy, adopts chemical soaking method Y (NO
3)
36H
2o solution impregnation pre-alloyed powder, through super-dry, hydrogen atmosphere protection heating makes it to be decomposed into Y
2o
3, thus obtain Y
2o
3dispersion strengthening ferrite type alloy powder, then carries out hot densification and prepares block materials.Chinese patent CN101823154A, discloses a kind of method adopting soaking method to prepare oxide dispersion strengthened iron powder, provides a kind of chemistry that fully utilizes and to infiltrate and the mechanical alloying of high-energy ball milling realizes the method for oxide dispersion strengthened iron powder.Chinese patent CN201110154483.7, disclose the preparation method of the dispersed particle-strengthened Alfer powdered steel of a kind of nano yttrium oxide, first ethylenediamine tetraacetic acid (EDTA) and chromium nitrate are added to the water, at least 12h is stirred at 50 ~ 60 DEG C, obtain mixed solution, in mixed solution, add citric acid, iron nitrate, ammonium paratungstate, Yttrium trinitrate and tetrabutyl titanate again, and stir at least 3h at 60 ~ 70 DEG C, obtain colloidal sol; Then, first in colloidal sol, add polyoxyethylene glycol, and be stirred to formation gel at 70 ~ 80 DEG C; Finally, at first successively gel being placed in 100 ~ 120 DEG C, drying at least 12h, roasting 4 ~ 5h at 300 ~ 600 DEG C, obtains oxidation of precursor thing powder, then is placed in reducing atmosphere, at least 3h is calcined, the obtained dispersed particle-strengthened Alfer powdered steel of nano yttrium oxide at 1100 ~ 1300 DEG C.
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, raw materials cost, the process costs of chemical powdering method are high, adopt a large amount of chemical reagent can introduce impurities left and pollution.
Ultrasonic disperse technology is generally applied to dispersion and the homogenizing of nano particle in colloidal dispersion.Nano-oxide particles easily forms colloid in a liquid, and micron-sized metallic powder particle is comparatively large, cannot form colloid in the solution.When directly utilizing the metal-powder in ultrasonic dispersed nano-oxide particles colloid, because metal powder granulates exists the difference of globule size, when metal-powder being added the nano-oxide particles colloidal solution of ultrasonic wave dispersion, oarse-grained metal powder cognition constantly adsorbs nano-oxide particles, causes occurring nano-oxide particles situation pockety.The macrobead metal base powder that early stage adds can absorb nano-oxide particles in a large number, and the iron powder macrobead then entered then only can adsorb remaining a small amount of nano-oxide particles, further increases the ununiformity of nano-oxide particles distribution.Therefore, directly utilize ultrasonic dispersed metal-powder and nano-oxide particles and nano-oxide particles is evenly attached on metal-powder and have difficulties.
Summary of the invention
The present invention is directed to existing machinery alloying and chemical method to prepare oxide dispersion intensifying iron and there is problems such as easily polluting, control process is complicated, oxide compound is easily reunited, a kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron is provided.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, comprises the following steps:
Nano-oxide powder is put into alcohol liquid, ultrasonic disperse is even, after obtaining suspension liquid, under ultrasonic disperse condition, progressively sends into suspension liquid, the bottom of iron-based powder from suspension liquid until iron-based powder is parallel with liquid level; Then drying obtains mixed powder; Finally, mixed powder press forming, sintering are obtained iron.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, described nano-oxide powder is TiO
2or Y
2o
3; Its granularity is less than or equal to 50nm.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, in described suspension liquid, nano-oxide particles concentration is 17g/L ~ 73g/L; Be preferably 17-50g/L, more preferably 17.5-45g/L.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, the ultrasonic frequency that ultrasonic disperse adopts is 20-40kHz.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, the granularity of described iron-based powder is less than or equal to 150 μm, is preferably less than or equal to 75 μm.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, the mass ratio of described iron-based powder and nano-oxide powder is 99.7:0.3 ~ 99:1.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, described alcohol liquid is selected from the one in the liquid alcohol such as dehydrated alcohol, anhydrous methanol, anhydrous propyl alcohol.In order to prevent iron powder surface oxidation, be beneficial to drying, recycling, the present invention selects conventional anhydrous alcohol solution simultaneously.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, suspension liquid is before adding iron-based powder, and sonic oscillation 15-25min, makes nano-oxide powder be uniformly dispersed.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, described iron-based powder is successively sent into suspension liquid from the bottom of suspension liquid, until iron-based powder is parallel with liquid level.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, in the process of adding iron-based powder, adopt and successively pave and hyperacoustic synergy, guarantee that the nano-oxide in liquid can not occur due to the difference in size of ferrous powder granules to reunite or flocculation.
The present invention, in powder feeding process, should keep hyperacoustic frequency and power, makes hyperacoustic acoustic density produce sufficient cavitation effect, to reach best dispersion effect.
The present invention is in powder feeding process, and the temperature of suspension liquid is room temperature.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, iron-based powder add complete after, keep ultra-sonic oscillation 5-10min, iron powder is made to be dispersed in nano-oxide particles suspension liquid, then reduce ultrasonic frequency and power gradually, hyperacoustic cavatition is progressively reduced, and particulate interspaces reduces gradually, avoid, because gravitational difference etc. acts on the phenomenons such as the absorption caused is uneven, realizing uniform settling absorption.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, described drying temperature is room temperature ~ 80 DEG C.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, the pressure of described press forming is 550-650MPa.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, during described sintering, controls vacuum tightness 10
-1-10
-2pa, temperature 1050-1200 DEG C, time 3-5h.
A kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron of the present invention, gained iron, through hot rolling and/or forge hot, obtains finished product; The temperature of described hot rolling and/or forge hot is 850-950 DEG C.
Advantage of the present invention and positively effect:
The bottom of iron-based powder from suspension liquid, under ultrasound condition, is successively sent into suspension liquid, until iron-based powder is parallel with liquid level by the present invention; Only can adsorb in the aspect of iron-based powder position when making iron-based powder enter suspension liquid and the nano-oxide of top close position, realize iron-based powder and successively adsorb nano-oxide, nano-oxide is uniformly distributed at iron-based powder; In addition, under the effect of ultrasonic energy, the nano-oxide less with iron-based powder bonding force, likely departs from the absorption of iron-based powder, reenters suspension liquid, is adsorbed by the follow-up iron-based powder entered, and effectively improves the homogeneity of nano-oxide distribution; On the other hand, ultrasonic vibration energy effectively can stop reunion between nano-oxide or flocculation, guarantees the homogeneity that nano-oxide distributes in iron-based powder.
When the present invention adds iron-based powder, keep former hyperacoustic frequency and power at 20-40Hz, be preferably about 30Hz, make hyperacoustic acoustic density produce sufficient cavitation effect, reach best dispersion effect.Meanwhile, suitable ultrasonic frequency can also impel the nano-oxide being about to reunite or flocculate to obtain dispersed, and this just further ensures the dispersion effect of nano-oxide.
When the present invention adds iron-based powder, suspension liquid temperature is room temperature, without the need to special control.Iron powder add complete after, keep ultra-sonic oscillation 5-10min, nano-oxide particles and iron powder are fully disperseed, reduce ultrasonic frequency gradually afterwards, hyperacoustic cavatition is slowly reduced, particulate interspaces reduces gradually, thus avoids because gravitational difference etc. acts on the phenomenons such as the absorption caused is uneven, realizes uniform settling absorption.
Present invention achieves the Homogeneous phase mixing of nano-oxide particles and iron-based powder, providing prerequisite for obtaining high quality disperse iron.
The invention solves the contingent agglomeration traits of disperse oxide, the disperse realizing nano-oxide is uniformly distributed; Overcome mechanical alloying and chemical method and prepare the shortcomings such as dispersed oxide easily pollutes, control process is complicated.
In a word, the present invention adopts and first disperses, decomposite technological line, namely ultrasonic disperse technology is utilized to be dispersed in room temperature liquid by nano-oxide particles, add iron-based powder again and make it mixing, final drying, makes nano-oxide particles be attached on iron-based powder; Utilize easy ultrasonic dispersion, realize effective depolymerization of nano-oxide particles in alcoholic solution, dispersed and distribution, obtained the dispersion-strengthened iron of superior performance by follow-up drying, compacting, sintering processes.Preparation technology of the present invention is simple, and nano-oxide particles disperse is effective, is suitable for large-scale industrial application.
Embodiment
Embodiment 1:
Preparation 0.5 (wt) %TiO
2dispersion-strengthened iron, its process is as follows:
(1) under ultrasound condition, granularity is less than or equal to the TiO of 10nm
2raw material powder (Detitanium-ore-type), add without in ethanolic soln, sonic oscillation 15min, makes TiO
2powder dispersion is even, obtain raw material powder concentration be 18g/L be suspended liquid, hyperacoustic frequency is 30kHz;
(2) under maintenance ultrasound condition, be less than or equal to the iron-based powder of 150 μm, at the uniform velocity handling powder feeding bottom vessel by granularity with funnel, successively tiling is to prepared being suspended in liquid, until iron-based powder is parallel with liquid level, obtains mixture; In the process of powder feeding, keep former hyperacoustic frequency and power, make hyperacoustic acoustic density produce sufficient cavitation effect, reach best dispersion effect, solution temperature remains on room temperature.Iron powder add complete after, keep ultra-sonic oscillation 8min, make iron powder be dispersed in nano-oxide particles alcohol suspending liquid, then reduce ultrasonic frequency and power gradually, until stop ultrasonic;
(3) to gained mixture after room temperature, normal pressure carry out drying treatment, through pressed compact, sintering obtain dispersion-strengthened iron.During pressed compact, control pressure is 550MPa; The condition of sintering is: vacuum tightness 10
-1-10
-2pa, temperature 1050 DEG C, time 3.5h.
(4) sintered body is carried out forge hot, forging temperature 850 DEG C, obtain nano-TiO
2dispersion strengthened iron.
Embodiment 2:
Preparation 1% (wt) Y
2o
3dispersion strengthened iron, its process is:
(1) configuration concentration is the Y of 36g/L
2o
3ethanolic soln, wherein Y
2o
3granularity is less than or equal to 30nm, and the soln using ultrasonoscope sonic oscillation 15min configured is made nanometer Y
2o
3be uniformly dispersed; Hyperacoustic frequency is 40kHz;
(2) under maintenance ultrasound condition, with funnel, granularity being less than or equal to the iron-based powder of 75 μm, being suspended liquid from the uniform velocity successively tiling bottom vessel to prepared, until iron-based powder upper surface reaches liquid level and parallel with liquid level; Keep ultra-sonic oscillation 10min; Then ultrasonic frequency and power is reduced gradually, until stop ultrasonic;
(3) mixture prepared by (2) step is inserted vacuum drying oven drying, drying temperature is 80 DEG C, time of drying 30min;
(4) dried mixed powder is inserted mould, adopt 600MPa pressure press forming, prepare the equally distributed pressed compact body of nano-oxide;
(5) pressed compact is inserted vacuum sintering furnace and carry out vacuum sintering, 1200 DEG C of sintering 1h, prepare the equally distributed sintered body of nano-oxide;
(6) sintered blank is carried out hot rolling shaping, hot-rolled temperature 950 DEG C, forging is fine and close obtains nanometer Y
2o
3dispersion strengthened iron.
Embodiment 3:
Preparation 0.5 (wt) %Y
2o
3dispersion strengthened iron, its process is:
(1) under ultrasound condition, granularity is less than or equal to the Y of-10nm
2o
3raw material powder, add in raw spirit liquid, sonic oscillation 15min, makes Y
2o
3powder dispersion is even, obtain raw material powder concentration be 18g/L be suspended liquid, hyperacoustic frequency is 30kHz;
(2) under maintenance ultrasound condition, be be less than or equal to the iron-based powder of 75 μm by granularity with funnel, being suspended liquid from the uniform velocity successively tiling bottom vessel to prepared, until iron-based powder upper surface reaches liquid level and parallel with liquid level, obtaining mixture; In the process of powder feeding, should keep former hyperacoustic frequency and power, make hyperacoustic acoustic density produce sufficient cavitation effect, reach best dispersion effect, solution temperature remains on room temperature.Iron powder add complete after, keep ultra-sonic oscillation 5min, make iron powder be dispersed in nano-oxide particles alcohol suspending liquid, then reduce ultrasonic frequency and power gradually, hyperacoustic cavatition is progressively reduced, until stop ultrasonic.
(3) to gained mixture after room temperature, normal pressure carry out drying treatment, through pressed compact, sintering obtain dispersion-strengthened iron.During pressed compact, control pressure is 600MPa; The condition of sintering is: vacuum tightness 10
-1-10
-2pa, temperature 1050 DEG C.
(4) sintered blank is carried out hot forging forming, forging temperature 900 DEG C, obtain nanometer Y
2o
3dispersion strengthened iron.
Claims (10)
1. the method adopting ultrasonic dispersion to prepare dispersion-strengthened iron, it is characterized in that: nano-oxide powder is put into alcohol liquid, ultrasonic disperse is even, after obtaining suspension liquid, under ultrasonic disperse condition, iron-based powder is sent into suspension liquid, until iron-based powder is parallel with liquid level from the bottom of suspension liquid; Then drying is uniformly mixed powder, then by mixed powder press forming, sintering, obtains iron.
2. a kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron according to claim 1, is characterized in that: the ultrasonic frequency that ultrasonic disperse adopts is 20-40kHz.
3. a kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron according to claim 1, is characterized in that: described nano-oxide powder is TiO
2or Y
2o
3; Its granularity is less than or equal to 50nm.
4. a kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron according to claim 1, it is characterized in that: in described suspension liquid, nano-oxide particles concentration is 17g/L ~ 73g/L.
5. a kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron according to claim 1, is characterized in that: the granularity of described iron-based powder is less than or equal to 150 μm; The mass ratio of described iron-based powder and nano-oxide powder is 99.7:0.3 ~ 99:1.
6. a kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron according to claim 1, is characterized in that: described alcohol liquid is selected from the one in dehydrated alcohol, anhydrous methanol, anhydrous propyl alcohol.
7. a kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron according to claim 1, is characterized in that: the temperature of suspension liquid is room temperature.
8. a kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron according to claim 1, is characterized in that: iron-based powder add complete after, keep ultra-sonic oscillation 5-10min.
9. a kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron according to claim 1, is characterized in that:
Described drying temperature is room temperature ~ 80 DEG C;
The pressure of described press forming is 550-650MPa;
During described sintering, control vacuum tightness 10
-1-10
-2pa, temperature 1050-1200 DEG C, time 3-5h.
10. a kind of method adopting ultrasonic dispersion to prepare dispersion-strengthened iron according to claim 1, is characterized in that: gained iron, through hot rolling or forge hot, obtains finished product; The temperature of described hot rolling or forge hot is 850-950 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115446302A (en) * | 2022-08-31 | 2022-12-09 | 鞍钢股份有限公司 | Iron-based intermediate with uniformly dispersed nanoparticles and preparation and use methods thereof |
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|---|---|---|---|---|
| US20210260651A1 (en) * | 2020-02-21 | 2021-08-26 | General Electric Company | Methods of manufacturing dispersion strengthened materials |
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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 |
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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 |
| 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 |
| CN103966500A (en) * | 2014-05-22 | 2014-08-06 | 北京航空航天大学 | ODS (ozone depleting substance) high temperature alloy added with composite oxide nanoparticles and preparation method thereof |
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2015
- 2015-03-10 CN CN201510104407.3A patent/CN104630602B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115446302A (en) * | 2022-08-31 | 2022-12-09 | 鞍钢股份有限公司 | Iron-based intermediate with uniformly dispersed nanoparticles and preparation and use methods thereof |
| 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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