CN104525962A - Method for preparing nanoscale oxide dispersion strengthening iron-based composite powder - Google Patents
Method for preparing nanoscale oxide dispersion strengthening iron-based composite powder Download PDFInfo
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- CN104525962A CN104525962A CN201410785487.9A CN201410785487A CN104525962A CN 104525962 A CN104525962 A CN 104525962A CN 201410785487 A CN201410785487 A CN 201410785487A CN 104525962 A CN104525962 A CN 104525962A
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Abstract
The invention relates to a method for preparing nanoscale oxide dispersion strengthening iron-based composite powder and belongs to the technical field of dispersion strengthening composite materials. The method is characterized by including the steps that ferric nitrate, a dispersed phase source, a reducing agent and an organic addition agent are prepared to be an even aqueous solution, the solution is heated, a precursor is obtained by volatilizing, concentrating and dissolving the solution, selective reduction is performed under the reducing atmosphere, and nanoscale oxide dispersion strengthening iron-based composite powder which is excellent in final product performance is obtained, wherein particles of dispersed phases are thin and small, and the dispersed phases are distributed uniformly and dispersedly. According to the method, raw materials are easily obtained, equipment is simple, the technological process is short, efficiency is high, cost is low, and the method is suitable for scale industrial production.
Description
Technical field
The invention belongs to dispersion strengthening composites preparing technical field, be specifically related to a kind of method preparing nano-scale oxide dispersion-strengtherning iron-based composite powder, the method raw material is easy to get, equipment is simple, technological process is short, efficiency is high, cost is low, be applicable to industrial production.
Technical background
Dispersion-strengtherning, solution strengthening, work hardening, refined crystalline strengthening are the Main Means of current raising material strong hardness.Wherein, dispersion-strengtherning has high-melting-point, high thermodynamic stability, high strong hardness and the at high temperature feature such as immiscible with matrix due to the second-phase of Dispersed precipitate, thus becomes a kind of important method very effectively improving material room temperature, high temperature strong hardness and high high-temp stability.The second-phase ultrafine particle that dispersion-strengtherning is mainly distributed by even dispersion carrys out the dislocation of pinning matrix, crystal boundary (sub boundary), hinder dislocation motion, prevent grain growth to play strengthening effect, in general, the distribution of wild phase particle dispersion is more even, and size is more tiny, and strengthening effect is better.The dispersion-strengtherning plasticity and toughness of not obvious reduction material and various physics again while significantly improving material strong hardness, thus make material obtain excellent combination property.Therefore, dispersion-strengtherning is a kind of more satisfactory strengthening means, shows larger development potentiality and wide application prospect, attracts the great interest of material supplier author, more become the study hotspot of material science.In recent years, the material such as dispersion-strengtherning high-performance copper base, iron-based, platinum base has been widely used in industrial every field.
In dispersion-strengtherning iron, oxide obtains extensive and deep research as the dispersion-strengthened material of wild phase, and has been widely used in the fields such as magnetic material, nuclear material, high-temperature material.Such as, in field of magnetic material, oxide dispersion intensifying iron is owing to both having higher magnetic conductivity, saturation induction density and low coercivity, there is again good room temperature mechanical behavior under high temperature simultaneously, thus become a kind of soft magnetic materials of excellent performance, now be widely used for producing various soft magnetism parts.In nuclear material field, dispersion-strengtherning iron belongs to BBC crystal structure, has the combination properties such as radioresistance, low swelling, anti-oxidant, anticorrosive, high creep strength, is used as the key structure materials such as nuclear reactor.
At present, the method preparing Oxide Dispersion Strengthened Materials Made mainly contains mechanical alloying method, internal oxidation etc.Chinese invention patent CN103331451A discloses a kind of mechanical alloying method and produces Al
2o
3the method of dispersion strengthening copper alloy powder, the method technique is simple, and consuming time short, made powder dispersity is good, but it is tiny not enough also to there is disperse phase, evenly, easily introduces the problems such as impurity; Chinese invention patent CN103451505A discloses a kind of method that internal oxidation prepares calcium oxide dispersion strengthened iron powder, the method has the tiny feature such as to be evenly distributed of disperse phase, but also there is technics comparing complexity, equipment requirement is high, is oxidized length consuming time and not easily prepares the equal problem of high-load disperse.Chinese invention patent CN101956119A discloses a kind of method that low-temperature combustion method prepares dispersion strengthened metal pre-alloyed powder, the method cost is low, equipment simple, the cycle is shorter, but, also there is matrix powder in the hot environment of burning easily to reunite and grow up, and then cause disperse phase also to be grown up thereupon, even occur segregation phenomenon, and reaction is than the stronger problem such as wayward.Therefore, in order to avoid the deficiency of said method, searching one can either be prepared disperse phase and be evenly distributed, and particle is tiny, and simple, that efficient, cost is low method becomes the task of top priority again simultaneously.
Summary of the invention
The present invention is directed to now methodical deficiency, specifically provide a kind of method preparing nano-scale oxide dispersion-strengtherning iron-based composite powder.This method avoid the deficiency of mechanical alloying method, internal oxidation, successfully solve again the powder existed in current combustion method easily to reunite and grow up and react problems such as being more acutely difficult to control, the method raw material is easy to get simultaneously, equipment is simple, technological process is short, efficiency is high, and cost is low, is applicable to industrial production.
The present invention is characterised in that and ferric nitrate, disperse phase source, reducing agent, organic additive is mixed with homogeneous aqueous solution, solution is heated to uniform temperature, solution generation redox reaction, obtain presoma, then carry out selective reduction under reducing atmosphere, obtain disperse phase and be evenly distributed, particle is tiny, dispersion, the nano-scale oxide dispersion-strengtherning iron-based composite powder of final products excellent performance.
The present invention introduces a kind of organic additive in the feed, its know-why is: organic additive has complexing, the complex compound with network structure can be formed with parent metal ion, dispersed phase metal ions and reducing agent in the solution, be conducive to the powder finally obtaining tiny dispersion; There is decomposition reaction, the additional heat produced in absorption reaction in additive simultaneously in the redox reaction of heat release, reduces reaction temperature, makes reaction become gentle controlled, stop powder to be reunited and grow up; In addition, additive produces additional gas when decomposing, and can powder be stoped further to reunite.
The present invention is characterised in that and comprises the following steps:
1) solution preparation: ferric nitrate, disperse phase source, reducing agent, organic additive are dissolved in deionized water according to a certain ratio, wiring solution-forming, wherein the mol ratio of reducing agent and metal ion in solution is (0.25 ~ 6): 1, and the mol ratio of organic additive and metal ion in solution is (0.05 ~ 2): 1;
2) preparation of presoma: solution is heated, solution evaporation, concentrated, decomposition, obtain precursor powder;
3) preparation of dispersion-strengtherning iron-based composite powder: under reducing atmosphere, is placed in presoma in stove, at 250 ~ 700 DEG C of reduction 0.5 ~ 4h, obtains dispersion-strengtherning iron-based composite powder.
Step 1) described in disperse phase source be yttrium nitrate, yttrium chloride, yttrium sulfate, aluminum nitrate, aluminium chloride, aluminum sulfate, in preparation process, ferric nitrate finally generates iron-based body through hydrogen reducing, disperse phase source is finally reduced and is generated disperse phase oxide, ferric nitrate and disperse phase source are rolled over respectively the quality of synthesis iron base body and disperse phase oxide, described disperse phase oxide mass accounts for 0.2% ~ 5% of iron-based body and disperse phase oxide gross mass;
Step 1) described in reducing agent be at least one in glycine, alanine, urea, citric acid, organic additive is at least one in glucose, sucrose, maltose;
Step 3) described in reducing atmosphere be the combination of at least one or itself and argon gas in hydrogen, cracked ammonium, optimum selective reduction temperature is 300 ~ 600 DEG C, and the optimum recovery time is 1 ~ 3h;
Prepared composite powder granularity is less than 50nm, is evenly distributed, favorable dispersibility.
The method has the following advantages:
1) utilize the fast reaction between each raw material in solution, in tens minutes, prepare precursor powder quickly and easily;
2) organic additive can form the complex compound with network structure, be conducive to the powder finally obtaining tiny dispersion, additive can decompose simultaneously, reduce reaction temperature, reaction is made to become gentle controlled, stop powder to be reunited to grow up, additive can also produce gas and can powder be stoped further to reunite in addition;
3) each composition Homogeneous phase mixing on a molecular scale can be realized in the solution, be conducive to being uniformly distributed of disperse phase in composite granule;
4) presoma activity is high, can reduce reduction reaction temperature, improves reaction speed;
5) the composite powder granularity prepared by is less than 50nm, is evenly distributed, favorable dispersibility, and can regulate and control the granularity of disperse phase particle and parent metal powder by feed change kind, proportioning, reduction reaction temperature and time;
6) raw material is easy to get, and equipment is simple, and technological process is short, and efficiency is high, and cost is low, is applicable to large-scale industrial and produces.
Accompanying drawing explanation
Fig. 1 is the XRD figure at yttria dispersion strengthening iron composite powder end prepared by the present invention;
Fig. 2 is the EDS figure at yttria dispersion strengthening iron composite powder end prepared by the present invention;
Fig. 3 is the SEM photo at yttria dispersion strengthening iron composite powder end prepared by the present invention;
Fig. 4 is the TEM photo at yttria dispersion strengthening iron composite powder end prepared by the present invention;
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further elaborated, should be understood that these embodiments are only not used in for illustration of the present invention and limit the scope of the invention.In addition should be understood that those skilled in the art can make various change or amendment to the present invention after the content of having read the present invention's instruction, these equivalences fall within the application's appended claims limited range equally.
Embodiment 1:0.5% yttria dispersion strengthening composite powder
Take 40.4g Fe (NO
3)
39H
2o, 0.095g Y (NO
3)
36H
2o, 7.507g glycine, 1.981g glucose, be dissolved in deionized water by various raw material, be mixed with solution; Be placed in by solution on controllable temperature electric furnace and heat, solution, after the series reaction such as experience volatilization, concentrated, decomposition, obtains precursor powder; In hydrogen atmosphere, precursor powder is inserted in stove, at 400 DEG C of reductase 12 h, obtain nano yttrium oxide dispersion-strengtherning iron-based composite powder.
Embodiment 2:1% yttria dispersion strengthening composite powder
Take 40.4g Fe (NO
3)
39H
2o, 0.129g Y (NO
3)
36H
2o, 9.008g glycine, 2.972g glucose, be dissolved in deionized water by various raw material, be mixed with solution; Be placed in by solution on controllable temperature electric furnace and heat, solution, after the series reaction such as experience volatilization, concentrated, decomposition, obtains precursor powder; In hydrogen atmosphere, precursor powder is inserted the inherent 500 DEG C of reductase 12 h of stove, obtain nano yttrium oxide dispersion-strengtherning iron-based composite powder.
Embodiment 3:2% yttria dispersion strengthening composite powder
Take 40.4g Fe (NO
3)
39H
2o, 0.387g Y (NO
3)
36H
2o, 8.909g alanine, 3.962g glucose, be dissolved in deionized water by various raw material, be mixed with solution; Be placed in by solution on controllable temperature electric furnace and heat, solution, after the series reaction such as experience volatilization, concentrated, decomposition, obtains precursor powder; In hydrogen atmosphere, precursor powder is inserted the inherent 600 DEG C of reduction 1h of stove, obtain nano yttrium oxide dispersion-strengtherning iron-based composite powder.
Embodiment 4:1% aluminum oxide dispersion strengthened iron base composite powder
Take 40.4g Fe (NO
3)
39H
2o, 0.415g Al (NO
3)
39H
2o, 6.060g urea, 2.972g glucose, be dissolved in deionized water by various raw material, be mixed with solution; Be placed in by solution on controllable temperature electric furnace and heat, solution, after the series reaction such as experience volatilization, concentrated, decomposition, obtains precursor powder; In hydrogen atmosphere, precursor powder is inserted the inherent 500 DEG C of reductase 12 h of stove, obtain nano yttrium oxide dispersion-strengtherning iron-based composite powder.
Embodiment 5:2% aluminum oxide dispersion strengthened iron base composite powder
Take 40.4g Fe (NO
3)
39H
2o, 0.838g Al (NO
3)
39H
2o, 9.607 citric acids, 3.962g glucose, be dissolved in deionized water by various raw material, be mixed with solution; Be placed in by solution on controllable temperature electric furnace and heat, solution, after the series reaction such as experience volatilization, concentrated, decomposition, obtains precursor powder; In hydrogen atmosphere, precursor powder is inserted the inherent 600 DEG C of reductase 12 h of stove, obtain nano yttrium oxide dispersion-strengtherning iron-based composite powder.
Claims (6)
1. prepare the method for nano-scale oxide dispersion-strengtherning iron-based composite powder, it is characterized in that comprising the steps:
1) solution preparation: ferric nitrate, disperse phase source, reducing agent, organic additive are dissolved in deionized water according to a certain percentage, wiring solution-forming, wherein the mol ratio of reducing agent and metal ion in solution is (0.25 ~ 6): 1, and the mol ratio of organic additive and metal ion in solution is (0.05 ~ 2): 1;
2) preparation of presoma: by step 1) the solution heating of preparing, solution evaporation, concentrated, decompose, obtain precursor powder;
3) preparation of dispersion-strengtherning iron-based composite powder: under reducing atmosphere, by step 2) presoma prepared is placed in stove, at 250 ~ 700 DEG C of reduction 0.5 ~ 4h, obtains dispersion-strengtherning iron-based composite powder.
2. the method preparing nano-scale oxide dispersion-strengtherning iron-based composite powder according to claim 1, it is characterized in that step 1) in disperse phase source be yttrium nitrate, yttrium chloride, yttrium sulfate, aluminum nitrate, aluminium chloride, aluminum sulfate, in preparation process, ferric nitrate finally generates iron-based body through hydrogen reducing, disperse phase source is finally reduced and is generated disperse phase oxide, ferric nitrate and disperse phase source are rolled over respectively the quality of synthesis iron base body and disperse phase oxide, described disperse phase oxide mass accounts for 0.2% ~ 5% of iron-based body and disperse phase oxide gross mass.
3. the method preparing nano-scale oxide dispersion-strengtherning iron-based composite powder according to claim 1, is characterized in that step 1) in reducing agent be at least one in glycine, alanine, urea, citric acid.
4. the method preparing nano-scale oxide dispersion-strengtherning iron-based composite powder according to claim 1, is characterized in that step 1) in organic additive be at least one in glucose, sucrose, maltose.
5. the method preparing nano-scale oxide dispersion-strengtherning iron-based composite powder according to claim 1, is characterized in that step 3) in reducing atmosphere be the combination of at least one or itself and argon gas in hydrogen, cracked ammonium.
6. the method preparing nano-scale oxide dispersion-strengtherning iron-based composite powder according to claim 1, is characterized in that step 3) in reduction temperature be 300 ~ 600 DEG C, the recovery time is 1 ~ 3h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104959624A (en) * | 2015-06-17 | 2015-10-07 | 北京科技大学 | Nanoscale oxide dispersion strengthened nickel base composite powder preparing method |
| CN109371308A (en) * | 2018-12-17 | 2019-02-22 | 湘潭大学 | The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end |
| CN113802042A (en) * | 2021-09-16 | 2021-12-17 | 北京科技大学 | Uniformly dispersed Al2O3Preparation method of/Fe composite material |
| CN113897528A (en) * | 2021-09-16 | 2022-01-07 | 北京科技大学 | Uniformly dispersed Fe-Ni/Al2O3Preparation method of magnetic composite material |
| CN113897529A (en) * | 2021-09-16 | 2022-01-07 | 北京科技大学 | Preparation method of rare earth oxide dispersion-strengthened iron-cobalt soft magnetic ultrafine crystal alloy |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010054328A1 (en) * | 2000-04-07 | 2001-12-27 | Korea Institute Of Machinery And Materials | Method of producing nanophase Cu-Al2O3 composite power |
| CN101837466A (en) * | 2010-04-02 | 2010-09-22 | 北京科技大学 | Method for preparing nano aluminum oxide dispersion iron powder |
| CN102690977A (en) * | 2012-04-17 | 2012-09-26 | 北京科技大学 | Method for preparing gamma' phase strengthened cobalt-based ODS alloy by using solution method |
| CN102814503A (en) * | 2011-06-09 | 2012-12-12 | 中国科学院合肥物质科学研究院 | Method for preparing dispersion strengthening ferritic alloy steel powder of nanometer yttrium oxide particles |
| CN102942226A (en) * | 2012-11-10 | 2013-02-27 | 南昌航空大学 | Preparation method for yttrium iron garnet powder |
| CN103008676A (en) * | 2013-01-15 | 2013-04-03 | 北京科技大学 | Method for manufacturing high-dispersion ultrafine molybdenum-based powder |
| CN103122420A (en) * | 2013-02-28 | 2013-05-29 | 北京科技大学 | Method for preparing porous nickel-based ODS ( Oxide Dispersion Strengthened) alloy |
-
2014
- 2014-12-17 CN CN201410785487.9A patent/CN104525962A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010054328A1 (en) * | 2000-04-07 | 2001-12-27 | Korea Institute Of Machinery And Materials | Method of producing nanophase Cu-Al2O3 composite power |
| CN101837466A (en) * | 2010-04-02 | 2010-09-22 | 北京科技大学 | Method for preparing nano aluminum oxide dispersion iron powder |
| CN102814503A (en) * | 2011-06-09 | 2012-12-12 | 中国科学院合肥物质科学研究院 | Method for preparing dispersion strengthening ferritic alloy steel powder of nanometer yttrium oxide particles |
| CN102690977A (en) * | 2012-04-17 | 2012-09-26 | 北京科技大学 | Method for preparing gamma' phase strengthened cobalt-based ODS alloy by using solution method |
| CN102942226A (en) * | 2012-11-10 | 2013-02-27 | 南昌航空大学 | Preparation method for yttrium iron garnet powder |
| CN103008676A (en) * | 2013-01-15 | 2013-04-03 | 北京科技大学 | Method for manufacturing high-dispersion ultrafine molybdenum-based powder |
| CN103122420A (en) * | 2013-02-28 | 2013-05-29 | 北京科技大学 | Method for preparing porous nickel-based ODS ( Oxide Dispersion Strengthened) alloy |
Non-Patent Citations (1)
| Title |
|---|
| 温玉仁 等: "纳米氧化物弥散强化铁素体合金的制备", 《粉末冶金材料科学与工程》, vol. 15, no. 1, 28 February 2010 (2010-02-28), pages 74 - 78 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104959624A (en) * | 2015-06-17 | 2015-10-07 | 北京科技大学 | Nanoscale oxide dispersion strengthened nickel base composite powder preparing method |
| CN109371308A (en) * | 2018-12-17 | 2019-02-22 | 湘潭大学 | The method for preparing multi-principal elements alloy toughened aluminum oxide base metal-ceramic composite powder end |
| CN113802042A (en) * | 2021-09-16 | 2021-12-17 | 北京科技大学 | Uniformly dispersed Al2O3Preparation method of/Fe composite material |
| CN113897528A (en) * | 2021-09-16 | 2022-01-07 | 北京科技大学 | Uniformly dispersed Fe-Ni/Al2O3Preparation method of magnetic composite material |
| CN113897529A (en) * | 2021-09-16 | 2022-01-07 | 北京科技大学 | Preparation method of rare earth oxide dispersion-strengthened iron-cobalt soft magnetic ultrafine crystal alloy |
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