CN101823152B - Method for preparing aluminum oxide dispersion strengthened iron pre-alloyed powder by using high-energy ball milling - Google Patents
Method for preparing aluminum oxide dispersion strengthened iron pre-alloyed powder by using high-energy ball milling Download PDFInfo
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- CN101823152B CN101823152B CN2010101486964A CN201010148696A CN101823152B CN 101823152 B CN101823152 B CN 101823152B CN 2010101486964 A CN2010101486964 A CN 2010101486964A CN 201010148696 A CN201010148696 A CN 201010148696A CN 101823152 B CN101823152 B CN 101823152B
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Abstract
The invention relates to a method for preparing oxide dispersion strengthened iron pre-alloyed powder by using high-energy ball milling and belongs to the field of oxide dispersion strengthened materials. The method comprises the following steps of: weighing a certain amount of Fe2O3 powder and dispersed phase oxide powder and ensuring that the content of the weighed oxide powder in an iron-oxide system is between 1 and 3 percent so as to ensure a dispersion strengthening effect; putting mixed powder into a planetary high-energy ball mill to perform ball milling for 20 to 40 hours excluding downtime, wherein machine halt is performed for 1 hour after every 5 hours of ball milling so as to prevent the temperature of a ball mill pot from getting too high; and reducing the ball-milled powder in hydrogen stream to obtain the oxide dispersion strengthened iron pre-alloyed powder because the Fe2O3 can be reduced by hydrogen while the dispersed phase oxide cannot be reduced by the hydrogen. The oxide dispersion strengthened iron pre-alloyed powder prepared by the method has small dispersed phase particles and is distributed uniformly. The method is simple to operate and easy to realize industrial production.
Description
Technical field
The invention belongs to oxide dispersion intensifying (Oxide Dispersion Strengthened; ODS) pre-alloyed powder preparing technical field provides a kind of method that adopts high-energy ball milling oxide and iron oxide mixed-powder to prepare aluminum oxide dispersion strengthened iron pre-alloyed powder especially.
Technical background
The fast breeder generating is the important development direction of following nuclear energy uses, and the fuel canning material of the low swelling low-activity of anti-irradiation is the important technological problems that fast reactor practicability must solve.The general fast reactor cladding materials of world the countries concerned is 316 austenitic stainless steels at present, and its swelling rate is higher, does not possess the long-life requirement.Ferritic steel has good anti-swelling property, but elevated temperature strength is relatively poor, has also limited its service life.And ODS (Oxide dispersion strengthened) type ferritic steel can increase substantially elevated temperature strength, has good anti-swelling performance again, is the preliminary election material that the fuel canning material long lifetime gets a good chance of.Powder metallurgical technique is mainly all adopted in the preparation of ODS ferritic steel at present, and wherein main component is oxide dispersion intensifying iron, and the preparation research of therefore carrying out oxide dispersion intensifying iron is very important.
The dispersion-strengtherning technology is highly effective means to heat endurance and hardness, the intensity that improves high temperature alloy particularly, also is the good method that common metal improves high-temperature behavior and mechanical property.The stable performance at high temperature of dispersed oxide phase particle; These disperses are distributed in oxide particle in the matrix can effectively improve alloy as the resistance of dislocation moving creep resisting ability and elevated temperature strength; In addition; Disperse is distributed in the carrying out that oxide particle in the matrix can hinder recrystallization process, obtains stable crystallite dimension easily.It is generally acknowledged that oxide particle is tiny more, it is even more to distribute, and the raising of material property is just remarkable more.Oxide dispersion intensifying is existing extremely successful application example in fields such as high property copper alloy, high temperature alloys.
At present, main mechanical alloying, the methods such as interior oxidation of adopting in the preparation of oxide dispersion intensifying material.The method that Chinese invention patent: CN200610128421.8 discloses a kind of interior oxidation prepares Al
2O
3Dispersion strengthening copper alloy materials.The method that Chinese invention patent: CN94112582.3 discloses a kind of mechanical ball milling alloying prepares the dispersion-strengthened copper electrode for upset welding material.Document 1 (material engineering, 1995,4:6) reported, be starting powder with Fe, with Cr, A-l, Ti, Mo is the intermediate alloy powder, with Y
2O
3(d＜50nm) be the second-phase dispersion enhanced particles, through mechanical alloying prepared high temperature alloy.Chinese invention patent: CN101535674A discloses the method that a kind of high-energy ball milling prepares oxide dispersion strengthened austenitic stainless steel.In its mechanical milling process; Disperse phase and metal dust mix, but because metal dust is harder, short time inner oxide disperse phase can not be wrapped up by metal dust; Can take place to reunite in the dispersed oxide phase powder process afterwards that is not wrapped to grow up, and then worsen the performance of material.
Summary of the invention
The object of the present invention is to provide a kind of method that adopts high-energy ball milling to prepare aluminum oxide dispersion strengthened iron pre-alloyed powder; Solve in traditional mechanical alloying mechanical milling process; Because metal dust is harder; Short time inner oxide disperse phase can not be wrapped up by metal dust, can take place to reunite in the dispersed oxide phase powder process afterwards that is not wrapped to grow up, and then worsen the problem of the performance of material.
A kind ofly prepare the method for oxide dispersion intensifying iron pre-alloyed powder with high-energy ball milling, its technical process is: take by weighing a certain amount of Fe
2O
3Powder and disperse phase oxide powder, the oxide powder that takes by weighing will guarantee that its content in iron-oxide system is 1-3%, to guarantee dispersion-strengthened effect.Put into the planetary high-energy ball mill ball milling to iron-oxide mixed-powder, ratio of grinding media to material is 10-12: 1, and drum's speed of rotation is 350-400r/min, the ball milling time is 20-40 hour, does not comprise downtime.Every ball milling was shut down 1 hour in 5 hours, and is too high to prevent the ball grinder temperature.Then that ball milling is good powder in hydrogen stream at 700-900 ℃ of reduction 40-60min, because Fe
2O
3Can be by hydrogen reducing and the disperse phase oxide can not, therefore obtain the oxide dispersion intensifying iron pre-alloyed powder at last.
This method is compared with traditional mechanical alloying, adopts Fe
2O
3Powder replaces metal Fe powder and the dispersed oxide common ball milling of powder mutually with the common ball milling of disperse phase oxide powder, because Fe
2O
3Powder is softer than Fe powder, and therefore in the process of high-energy ball milling, disperse phase enters into Fe more easily
2O
3In the powder and then by Fe
2O
3Powder wraps up, resulting disperse phase more even distribution, and the disperse phase oxide powder that is wrapped can not reunited with other disperse phase oxide powder in mechanical milling process, has suppressed growing up of disperse phase, resulting disperse phase particle is tiny.
The specific embodiment
Embodiment 1:1%Al
2O
3The dispersion strengthened iron powder
Testing used raw material is Fe
2O
3Powder and Al
2O
3Powder, the purity of using powder be all greater than 99.9%, wherein Fe
2O
3The granularity of powder is 10 μ m, Al
2O
3The granularity of powder is 30nm.Take by weighing a certain amount of Fe
2O
3Powder and Al
2O
3Powder guarantees Al
2O
3At Fe-Al
2O
3Content in the system is 1%.Put into the planetary high-energy ball mill ball milling to mixed-powder, ratio of grinding media to material is 10: 1, and the rotating speed of ball mill is 350r/min, and the ball milling time was controlled at 40 hours, did not comprise downtime.Every ball milling was shut down 1 hour in 5 hours, and is too high to prevent the ball grinder temperature.Then that ball milling is good powder at 700 ℃ of reduction 60min, obtains Al at last in hydrogen stream
2O
3Dispersion strengthened iron pre-alloyed powder.
Embodiment 2:2%Al
2O
3The dispersion strengthened iron powder
Testing used raw material is Fe
2O
3Powder and Al
2O
3Powder, the purity of using powder be all greater than 99.9%, wherein Fe
2O
3The granularity of powder is 10 μ m, Al
2O
3The granularity of powder is 30nm.Take by weighing a certain amount of Fe
2O
3Powder and Al
2O
3Powder guarantees Al
2O
3At Fe-Al
2O
3Content in the system is 2%.Put into the planetary high-energy ball mill ball milling to mixed-powder, ratio of grinding media to material is 11: 1, and the rotating speed of ball mill is 380r/min, and the ball milling time was controlled at 30 hours, did not comprise downtime.Every ball milling was shut down 1 hour in 5 hours, and is too high to prevent the ball grinder temperature.Then that ball milling is good powder at 800 ℃ of reduction 50min, obtains Al at last in hydrogen stream
2O
3Dispersion strengthened iron pre-alloyed powder.
Embodiment 3:3%Y
2O
3The dispersion strengthened iron powder
Testing used raw material is Fe
2O
3Powder and Y
2O
3Powder, the purity of using powder be all greater than 99.9%, wherein Fe
2O
3The granularity of powder is 10 μ m, Y
2O
3The granularity of powder is 30nm.Take by weighing a certain amount of Fe
2O
3Powder and Y
2O
3Powder guarantees Y
2O
3At Fe-Y
2O
3Content in the system is 3%.Put into the planetary high-energy ball mill ball milling to mixed-powder, ratio of grinding media to material is 12: 1, and the rotating speed of ball mill is 400r/min, and the ball milling time was controlled at 20 hours, did not comprise downtime.Every ball milling was shut down 1 hour in 5 hours, and is too high to prevent the ball grinder temperature.Then that ball milling is good powder at 900 ℃ of reduction 40min, obtains Y at last in hydrogen stream
2O
3Dispersion strengthened iron pre-alloyed powder.
Claims (1)
1. a method that adopts high-energy ball milling to prepare aluminum oxide dispersion strengthened iron pre-alloyed powder is characterized in that technical process is: take by weighing a certain amount of Fe
2O
3Powder and disperse phase oxide powder, the oxide powder that takes by weighing will guarantee that its weight percent content in iron-oxide system is 1-3%, to guarantee dispersion-strengthened effect; Put into the planetary high-energy ball mill ball milling to iron-oxide mixed-powder, ratio of grinding media to material is 10-12: 1, and drum's speed of rotation is 350-400r/min, the ball milling time is 20-40 hour, does not comprise downtime; Every ball milling 5 hours was shut down 1 hour, then that ball milling is good powder in hydrogen stream at 700-900 ℃ of reduction 40-60min, because Fe
2O
3Can be by hydrogen reducing and the disperse phase oxide can not, therefore obtain the oxide dispersion intensifying iron pre-alloyed powder at last; Used oxide is Al
2O
3, can not be by hydrogen reducing.
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|---|---|---|---|
| CN2010101486964A CN101823152B (en) | 2010-04-14 | 2010-04-14 | Method for preparing aluminum oxide dispersion strengthened iron pre-alloyed powder by using high-energy ball milling |
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| CN2010101486964A CN101823152B (en) | 2010-04-14 | 2010-04-14 | Method for preparing aluminum oxide dispersion strengthened iron pre-alloyed powder by using high-energy ball milling |
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| Publication Number | Publication Date |
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| CN101823152A CN101823152A (en) | 2010-09-08 |
| CN101823152B true CN101823152B (en) | 2012-06-06 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102407336A (en) * | 2010-09-25 | 2012-04-11 | 李国平 | Method for preparing partially pre-alloyed iron powder by short process |
| CN102127713B (en) * | 2011-02-22 | 2012-06-06 | 中南大学 | Oxide dispersion-strengthening ferrite steel with bicrystal structure and production method thereof |
| CN102127712B (en) * | 2011-02-22 | 2012-08-08 | 中南大学 | Micro alloyed oxide dispersion-strengthening ferrite steel and preparation method |
| CN102127714A (en) * | 2011-02-22 | 2011-07-20 | 中南大学 | Nano-cluster-strengthened iron-base superalloy |
| CN103203457A (en) * | 2013-04-15 | 2013-07-17 | 河北钢铁股份有限公司邯郸分公司 | Method for manufacturing iron-copper alloy from iron oxide red and copper sulfate |
| CN103817340A (en) * | 2014-03-13 | 2014-05-28 | 抚顺龙诚新科技材料有限公司 | Preparation method for superfine pre-alloyed powder |
| CN104148661B (en) * | 2014-09-03 | 2016-01-06 | 湖北鄂信钻石科技股份有限公司 | A kind of preparation method of aluminum oxide dispersion prealloy powder |
| CN104493192A (en) * | 2014-12-17 | 2015-04-08 | 上海寰保渣业处置有限公司 | Micron-sized ultrafine iron powder preparation method |
| CN109550964A (en) * | 2017-09-27 | 2019-04-02 | 鞍钢股份有限公司 | A kind of preparation method of dispersion strengthening iron-base alloy powder |
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| CN1042807C (en) * | 1994-10-26 | 1999-04-07 | 中国科学院金属研究所 | Dispersion-strengthened copper electrode for upset welding |
| KR101319870B1 (en) * | 2006-01-05 | 2013-10-18 | 엘지전자 주식회사 | Method for handover in mobile communication system |
| CN101250639B (en) * | 2008-03-27 | 2010-08-18 | 哈尔滨工业大学深圳研究生院 | Novel nanometer phase dispersion strengthening cuprum as well as preparation method and product producing technique thereof |
| CN101386076A (en) * | 2008-10-24 | 2009-03-18 | 北京科技大学 | Preparation method of prealloy powder for nano level oxide dispersion strengthened metal |
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