CN101823154A - Method for preparing oxide dispersion strengthened iron powder by infiltration method - Google Patents
Method for preparing oxide dispersion strengthened iron powder by infiltration method Download PDFInfo
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- CN101823154A CN101823154A CN 201010148586 CN201010148586A CN101823154A CN 101823154 A CN101823154 A CN 101823154A CN 201010148586 CN201010148586 CN 201010148586 CN 201010148586 A CN201010148586 A CN 201010148586A CN 101823154 A CN101823154 A CN 101823154A
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Abstract
The invention relates to a method for preparing oxide dispersion strengthened iron powder by an infiltration method 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 chemically soaking the Fe2O3 powder; soaking the Fe2O3 powder in dispersed phase metallic ion nitrate solution; drying a soaked mixture at a low temperature and performing ball milling on the dried mixture in a high energy ball mill for a certain period of time; fully mixing dispersed phase metallic ion salt and Fe2O3; calcining the mixture in a muffle furnace at a high temperature to decompose dispersed phase metallic nitrate into a dispersed phase oxide so as to obtain mixed superfine oxide powder; reducing the obtained mixed oxide powder in a hydrogen furnace to obtain pre-alloyed powder which is prepared by uniformly mixing nano-scale oxide particles and nano-iron metallic particles because the dispersed phase oxide cannot be reduced by hydrogen. The method has the characteristics of simple operation, easy industrial production, capability of realizing uniform distribution of dispersed phases and small particle sizes of dispersed phase particles.
Description
Technical field
The invention belongs to the Oxide Dispersion Strengthened Materials Made field, provide especially a kind of and fully utilized that chemistry infiltrates and the mechanical alloying of high-energy ball milling prepares the method for oxide dispersion strengthened iron powder.
Technical background
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.It is generally acknowledged that oxide particle is more tiny, it is more even to distribute, and the raising of material property is just more remarkable.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 Strengthened Materials Made.The method that Chinese invention patent: CN200610128421.8 discloses a kind of interior oxidation prepares the Al2O3 dispersion 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, Al, Ti, Mo are the intermediate alloy powder, (d＜50nm) is the second-phase dispersion enhanced particles, prepares high temperature alloy by the mechanical alloy metallization processes with Y2O3.
Patent: CN1664145A discloses the method that the chemical infusion method of a kind of usefulness is made oxide dispersion strengthening ferrite type alloy.Adopt chemical infusion method Y (NO
3)
36H
2O solution impregnation prealloy powder guarantees the Y that finally obtains
2O
3Mass fraction in alloyed powder is 0.2-0.5%.Through super-dry, hydrogen atmosphere protection heating makes Y (NO
3)
36H
2O is decomposed into Y
2O
3Thereby, obtain Y
2O
3Dispersion strengthening ferrite type alloy.Adopt this method in the process that infiltrates, the granular size of disperse phase and uniformity coefficient are limited by the amount of solution used when infiltrating to a great extent.It is not saturating that solution is crossed infiltration at least, causes disperse phase inhomogeneous; Solution is crossed and can be made the disperse skew poly-at most, causes oarse-grained generation.
Summary of the invention
The object of the present invention is to provide and a kind ofly fully utilize that chemistry infiltrates and high-energy ball milling prepares the method for oxide dispersion strengthened iron powder, it is not enough even to have overcome in the mechanical alloying method disperse degree, do not reach the shortcomings such as high performance requirements, solved simultaneously the granular size of disperse phase in the simple employing infusion method and the problem that uniformity coefficient is limited by the amount of solution used when infiltrating.
A kind of method that adopts infusion method to prepare oxide dispersion strengthened iron powder is got earlier a certain amount of Fe
2O
3Powder adopts chemistry to infiltrate, Fe
2O
3Powder is positioned in the dispersed phase metal ions nitrate solution and infiltrates, and puts into high energy ball mill ball milling certain hour then after infiltrating good mixture low temperature drying, allows dispersed phase metal ions nitrate and Fe
2O
3Fully mix, take out afterwards and put into the Muffle furnace high-temperature calcination after low temperature drying a period of time and make the disperse phase metal nitrate be decomposed into the disperse phase oxide, obtain the superfine oxide mixed-powder; The disperse phase oxide oxide mixed-powder of gained reduced in hydrogen furnace, owing to can not by hydrogen reducing, obtain nano-scale oxide particle and the mixed uniformly pre-alloyed powder of nanometer matrix metallic particles at last.The concrete operations step is as follows:
1) configuration concentration is the disperse phase metal-nitrate solutions of 0.01-0.1mol/L, and the disperse phase metal-nitrate solutions that configures is joined Fe
2O
3In the powder;
2) will fully soak into good powder and put into baking oven in 80-100 ℃ of low temperature drying;
3) put into a certain amount of steel ball in ball grinder, the mixture after the oven dry is put into ball grinder, making ratio of grinding media to material is 10-15: 1, place ball milling 30-40h on the high energy ball mill then, and the rotating speed of ball mill is 240-300r/min;
4) powder behind the ball milling is put into Muffle furnace 300-500 ℃ of calcining, made the disperse phase metal nitrate be decomposed into the disperse phase oxide, obtain the superfine oxide mixed-powder;
5) mixed-powder is placed hydrogen behind 700-900 ℃ of reduction 40-60min, generate the mixed-powder of disperse phase oxide and iron powder, promptly nano-scale dispersion-strengthened iron powder.
The addition of dispersed phase metal ions nitrate solution will guarantee that the disperse phase oxide accounts for the 1-3% of nano-scale dispersion-strengthened iron powder weight, to guarantee strengthening effect.
Principle of the present invention is: yttrium nitrate solution is with after iron oxide mixes, because croci is tiny, specific area is big, plays the effect of absorption, yttrium nitrate and iron oxide are fully mixed, under the effect of high-energy ball milling, yttrium nitrate further mixes with iron oxide, and in the process of high-energy ball milling, because the fragmentation of high-energy ball milling, the yttrium nitrate crystal is broken and comes, and the yttria particles that calcining obtains later can not grown up, and particle is tiny evenly.
The invention has the advantages that the advantage that infiltrates in conjunction with high-energy ball milling and chemistry, can effectively reduce the formation of big yttria particles, the disperse phase of formation is tiny and be evenly distributed.Owing to after chemistry infiltrates, added a step high-energy ball milling, effectively avoided adopting the granular size of disperse phase in the chemical infusion method and the problem that uniformity coefficient is limited by the amount of solution used when infiltrating.
The specific embodiment
Embodiment 1:1%Y
2O
3The dispersion strengthened iron powder
(1) configuration concentration is the yttrium nitrate solution of 0.01mol/L, and the yttrium nitrate solution that configures is joined Fe
2O
3Make the Y that decomposites in the powder
2O
3Account for 1% of nano-scale dispersion-strengthened iron powder weight;
(2) will fully soak into good powder and put into baking oven in 80 ℃ of low temperature dryings;
(3) put into a certain amount of steel ball in ball grinder, the mixture after the oven dry is put into ball grinder, making ratio of grinding media to material is 10: 1, places ball milling 30h on the high energy ball mill then, and the rotating speed of ball mill is 240r/min;
(4) powder behind the ball milling is put into Muffle furnace 300 ℃ of calcinings, obtained the superfine oxide mixed-powder;
(5) mixed-powder is placed hydrogen behind 700 ℃ of reduction 60min, can obtain nanoscale disperse phase and strengthen iron powder.
Embodiment 2:2%Al
2O
3The dispersion strengthened iron powder
(1) configuration concentration is the aluminum nitrate solution of 0.05mol/L, and the aluminum nitrate solution that configures is joined Fe
2O
3Make the Al that decomposites in the powder
2O
3Account for 2% of nano-scale dispersion-strengthened iron powder weight;
(2) will fully soak into good powder and put into baking oven in 90 ℃ of low temperature dryings;
(3) put into a certain amount of steel ball in ball grinder, the mixture after the oven dry is put into ball grinder, making ratio of grinding media to material is 12: 1, places ball milling 35h on the high energy ball mill then, and the rotating speed of ball mill is 270r/min;
(4) powder behind the ball milling is put into Muffle furnace 400 ℃ of calcinings, obtained the superfine oxide mixed-powder;
(5) mixed-powder is placed hydrogen behind 800 ℃ of reduction 50min, can obtain nanoscale disperse phase and strengthen iron powder.
Embodiment 3:3%Y
2O
3The dispersion strengthened iron powder
(1) configuration concentration is the yttrium nitrate solution of 0.1mol/L, and the yttrium nitrate solution that configures is joined Fe
2O
3Make the Y that decomposites in the powder
2O
3Account for 3% of nano-scale dispersion-strengthened iron powder weight;
(2) will fully soak into good powder and put into baking oven in 100 ℃ of low temperature dryings;
(3) put into a certain amount of steel ball in ball grinder, the mixture after the oven dry is put into ball grinder, making ratio of grinding media to material is 15: 1, places ball milling 40h on the high energy ball mill then, and the rotating speed of ball mill is 300r/min;
(4) powder behind the ball milling is put into Muffle furnace 500 ℃ of calcinings, obtained the superfine oxide mixed-powder;
(5) mixed-powder is placed hydrogen behind 900 ℃ of reduction 40min, can obtain nanoscale disperse phase and strengthen iron powder.
Claims (2)
1. a method that adopts infusion method to prepare oxide dispersion strengthened iron powder is characterized in that: get earlier a certain amount of Fe
2O
3Powder adopts chemistry to infiltrate, Fe
2O
3Powder is positioned in the dispersed phase metal ions nitrate solution and infiltrates, and puts into high energy ball mill ball milling certain hour then after infiltrating good mixture low temperature drying, allows dispersed phase metal ions salt and Fe
2O
3Fully mix, put into afterwards the Muffle furnace high-temperature calcination and make the disperse phase metal nitrate be decomposed into the disperse phase oxide, obtain the superfine oxide mixed-powder; The disperse phase oxide oxide mixed-powder of gained reduced in hydrogen furnace, owing to can not by hydrogen reducing, obtain nano-scale oxide particle and the mixed uniformly pre-alloyed powder of nanometer matrix metallic particles at last; Concrete operation step is as follows:
1) configuration concentration is the disperse phase metal-nitrate solutions of 0.01-0.1mol/L, and the disperse phase metal-nitrate solutions that configures is joined Fe
2O
3In the powder;
2) will fully infiltrate good Fe
2O
3Powder is put into baking oven and is obtained mixture in 80-100 ℃ of low temperature drying;
3) put into a certain amount of steel ball in ball grinder, the mixture after the oven dry is put into ball grinder, making ratio of grinding media to material is 10-15: 1, place then that ball milling 30-40h obtains powder on the high energy ball mill, and the rotating speed of ball mill is 240-300r/min;
4) powder behind the ball milling is put into Muffle furnace 300-500 ℃ of calcining, made the disperse phase metal nitrate be decomposed into the disperse phase oxide, obtain the superfine oxide mixed-powder;
5) mixed-powder is placed hydrogen behind 700-900 ℃ of reduction 40-60min, generate the mixed-powder of disperse phase oxide and iron powder, promptly nano-scale dispersion-strengthened iron powder;
The addition of dispersed phase metal ions nitrate solution will guarantee that the disperse phase oxide accounts for the 1-3% of nano-scale dispersion-strengthened iron powder weight, to guarantee strengthening effect.
2. according to the described a kind of method that adopts infusion method to prepare oxide dispersion strengthened iron powder of claim 1, it is characterized in that: dispersed phase metal ions nitrate is aluminum nitrate or yttrium nitrate.
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| CN101823154B CN101823154B (en) | 2012-01-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091788A (en) * | 2010-11-23 | 2011-06-15 | 北京科技大学 | Method for industrially producing iron-based dispersion-strengthened material with low cost on large scale |
| CN102114543A (en) * | 2011-03-23 | 2011-07-06 | 北京矿冶研究总院 | Preparation and spraying method of aluminum bronze powder containing dispersion strengthening phase |
| CN108274010A (en) * | 2018-03-05 | 2018-07-13 | 无锡市福莱达石油机械有限公司 | Reduce the preparation method of carbide oxidation and decarbonization hot spray powder |
Citations (2)
| 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 |
| 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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2010
- 2010-04-14 CN CN2010101485868A patent/CN101823154B/en not_active Expired - Fee Related
Patent Citations (2)
| 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 |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 《北京科技大学学报》 19970831 彭顺米等 化学浸润法氧化物弥散强化铁素体合金的静态再结晶 346-350 1-2 第19卷, 第4期 2 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091788A (en) * | 2010-11-23 | 2011-06-15 | 北京科技大学 | Method for industrially producing iron-based dispersion-strengthened material with low cost on large scale |
| CN102091788B (en) * | 2010-11-23 | 2013-07-17 | 北京科技大学 | Method for industrially producing iron-based dispersion-strengthened material |
| CN102114543A (en) * | 2011-03-23 | 2011-07-06 | 北京矿冶研究总院 | Preparation and spraying method of aluminum bronze powder containing dispersion strengthening phase |
| CN108274010A (en) * | 2018-03-05 | 2018-07-13 | 无锡市福莱达石油机械有限公司 | Reduce the preparation method of carbide oxidation and decarbonization hot spray powder |
| CN108274010B (en) * | 2018-03-05 | 2021-05-11 | 无锡市福莱达石油机械有限公司 | Preparation method of thermal spraying powder for reducing oxidation and decarbonization of carbide |
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| CN101823154B (en) | 2012-01-25 |
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