CN104874807A - Preparation method for nanometer iron-cobalt solid solution alloy powder with body-centered cubic structure - Google Patents
Preparation method for nanometer iron-cobalt solid solution alloy powder with body-centered cubic structure Download PDFInfo
- Publication number
- CN104874807A CN104874807A CN201510338295.8A CN201510338295A CN104874807A CN 104874807 A CN104874807 A CN 104874807A CN 201510338295 A CN201510338295 A CN 201510338295A CN 104874807 A CN104874807 A CN 104874807A
- Authority
- CN
- China
- Prior art keywords
- cobalt
- alloy powder
- preparation
- centered cubic
- solid solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a preparation method for nanometer iron-cobalt solid solution alloy powder with a body-centered cubic structure and belongs to the field of nanometer metal powder preparation. The preparation method for the nanometer iron-cobalt solid solution alloy powder with the body-centered cubic structure includes that firstly, dissolving ferric nitrate, cobalt nitrate, reducing agent and complexing agent in de-ionized water according to a certain proportion to prepare into solution, and heating the solution till occurring a vigorous oxidation reduction reaction to obtain nanometer iron-cobalt oxide precursor powder; secondly, reducing the precursor powder in a hydrogen or cracked ammonia atmosphere to obtain the nanometer iron-cobalt solid solution alloy powder with the body-centered cubic structure, wherein the reducing temperature is 300 to 900 degrees centigrade, and the reducing time is 1 to 3 hours. The nanometer alloy powder is stable in performance, reliable in quality and high in saturated magnetic induction density. The preparation method is broad in raw material source, simple in equipment, short in technique, low in cost, good in safety, stable in production quality, high in efficiency and capable of realizing large-scale production, and a new thinking is provided for preparing the high-performance nanometer iron-cobalt alloy powder.
Description
Technical field
The present invention relates to a kind of preparation method with body-centered cubic structure Nanoscale Iron cobalt solid solution alloy powder, belong to nano metal powder preparation field.
Background technology
Iron cobalt Magnaglo is owing to having higher saturation induction density and higher Curie temperature and have extensive use in data storing, Magnetic resonance imaging etc.Purity, the crystallite dimension of iron cobalt Magnaglo are the key factors affecting iron cobalt magnetic material with thing mutually.In general purity is high, crystal grain tiny (<100nm) and the Nanoscale Iron cobalt solid-solution powder with body-centered cubic structure (bcc) has the highest saturation induction density.The existing method preparing Nanoscale Iron cobalt magnetic material mainly contains high-energy ball milling method, chemical reaction ball-milling method and solution chemical method.These methods can successfully prepare Nanoscale Iron cobalt alloy powder, but also have its defect.During as high-energy ball milling method and reaction ball milling method consumption energy consumption, be not suitable for scale preparation, mechanical milling process very easily introduces impurity or stress in Nanoscale Iron cobalt alloy simultaneously, thus reduces the saturation induction density of Nanoscale Iron cobalt alloy.Solution chemical method can prepare the Nanoscale Iron cobalt alloy powder of various pattern and size very easily; but existing prepare Nanoscale Iron cobalt alloy powder solution chemical method otherwise need the reaction that uses poisonous raw material to carry out the long period, or remain surfactant or other protective layers at the particle surface of preparation and have impact on the magnetic property of Nanoscale Iron cobalt alloy.Therefore be necessary to introduce a kind of efficient, nontoxic and do not need to use the method for surfactant additive to prepare Nanoscale Iron cobalt alloy powder.
Summary of the invention
The object of the present invention is to provide a kind of method preparing Nanoscale Iron cobalt alloy powder, be intended to use poisonous material to prepare and there is body-centered cubic structure Nanoscale Iron cobalt solid solution alloy powder.
First the present invention prepares the nanometer precursor powder of iron content, cobalt element, in hydrogen or cracked ammonium atmosphere, then carry out precursor powder to reduce the Nanoscale Iron cobalt solid solution alloy powder obtaining having body-centered cubic structure.As shown in Figure 1, concrete steps are as follows for preparation technology:
1) solwution method prepares nano-oxide precursor powder: ferric nitrate, cobalt nitrate, reducing agent and complexing agent are dissolved in deionized water by a certain percentage, wiring solution-forming, heated solution, until there is vigorous oxidation reduction reaction, obtains Nanoscale Iron cobalt/cobalt oxide precursor powder.Wherein, reducing agent is at least one in urea, glycine, and the mol ratio of itself and ferric nitrate is (0.05 ~ 3): 1; Complexing agent is at least one in glucose, citric acid and tetraacethyl diaminoethanes (EDTA), and the mol ratio of itself and ferric nitrate is (0.5 ~ 1.5): 1; In target Nanoscale Iron cobalt alloy powder, the ratio of iron cobalt is determined by the ratio of ferric nitrate in raw material and cobalt nitrate, the mass fraction 30 ~ 70% of iron in general warranty target Nanoscale Iron cobalt alloy powder, the mass fraction 70 ~ 30% of cobalt.
In redox reaction, reducing agent is organic-fuel, provides the N of+5 valencys in the N element of-3 valencys and nitrate that violent redox reaction occurs, and according to the ratio of reducing agent and nitrate, can generate N in course of reaction
2, CO
2, NO, NO
2deng gas, a large amount of gas can prevent precursor powder from reuniting; The effect of complexing agent is the metal ion in complex reaction system, prevents the hydrolytic precipitation of metal ion in solution, provides part reaction energy simultaneously and increases gas yield, preventing precursor powder from reuniting further.
2) reduce: reduced in hydrogen or cracked ammonium atmosphere by the precursor powder obtained, reduction temperature is 300 ~ 900 DEG C, and the recovery time is 1 ~ 3 hour, obtains the Nanoscale Iron cobalt solid solution alloy powder with body-centered cubic structure.As shown in Figure 2, the TEM shape appearance figure of Nanoscale Iron cobalt alloy powder as shown in Figure 3 for the X-ray diffraction analysis figure of Nanoscale Iron cobalt alloy powder.Prepared Nanoscale Iron cobalt alloy powder properties of product are stable, reliable in quality, saturation induction density are high.
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) each composition Homogeneous phase mixing on a molecular scale can be realized in the liquid phase, be conducive to being uniformly distributed of iron cobalt element in iron cobalt solid solution alloy;
3) presoma activity is high, can reduce reduction temperature, Reaction time shorten;
4) the alloy nano-powder purity prepared by is high, and powder diameter is little, good dispersion, and can regulate and control the size of powder particle by feed change kind, proportioning, reduction temperature and time;
5) 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, for the preparation of high-performance nano iron cobalt solid solution alloy powder provides new thinking.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention
Fig. 2 is the X-ray diffraction analysis figure of Nanocrystalline Cobalt alloy powder
Fig. 3 is the TEM shape appearance figure of Nanocrystalline Cobalt alloy powder
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further elaborated.These embodiments should be understood only be 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: crystallite dimension is the body-centered cubic structure Fe of 50nm
50co
50the preparation of solid solution alloy powder
Nine water ferric nitrates, cobalt nitrate hexahydrate, glycine and glucose are dissolved in deionized water by a certain percentage, wiring solution-forming, heated solution is to vigorous oxidation reduction reaction occurs, obtain Nanoscale Iron cobalt/cobalt oxide precursor powder, wherein the mol ratio of cobalt nitrate hexahydrate and nine water ferric nitrates is 0.95:1, the mol ratio of glycine and nine water ferric nitrates is 2:1, and the mol ratio of glucose and nine water ferric nitrates is 0.6:1; By precursor powder reductase 12 hour in hydrogen atmosphere at 700 DEG C, obtain the body-centered cubic structure Fe that crystallite dimension is 50nm
50co
50solid solution alloy powder.
Embodiment 2: crystallite dimension is the body-centered cubic structure Fe of 30nm
50co
50the preparation of solid solution alloy powder
Nine water ferric nitrates, cobalt nitrate hexahydrate, glycine and glucose are dissolved in deionized water by a certain percentage, wiring solution-forming, heated solution is to vigorous oxidation reduction reaction occurs, obtain Nanoscale Iron cobalt/cobalt oxide precursor powder, wherein the mol ratio of cobalt nitrate hexahydrate and nine water ferric nitrates is 0.95:1, the mol ratio of glycine and nine water ferric nitrates is 1.5:1, and the mol ratio of glucose and nine water ferric nitrates is 0.8:1; Precursor powder is reduced 1 hour in hydrogen atmosphere at 300 DEG C, obtains the body-centered cubic structure Fe that crystallite dimension is 30nm
50co
50solid solution alloy powder.
Embodiment 3: crystallite dimension is the body-centered cubic structure Fe of 60nm
50co
50the preparation of solid solution alloy powder
Nine water ferric nitrates, cobalt nitrate hexahydrate, urea and citric acid are dissolved in deionized water by a certain percentage, wiring solution-forming, heated solution is to vigorous oxidation reduction reaction occurs, obtain Nanoscale Iron cobalt/cobalt oxide precursor powder, wherein the mol ratio of cobalt nitrate hexahydrate and nine water ferric nitrates is 0.95:1, the mol ratio of urea and nine water ferric nitrates is 0.5:1, and the mol ratio of citric acid and nine water ferric nitrates is 1.2:1; By precursor powder reductase 12 hour in cracked ammonium atmosphere at 650 DEG C, obtain the body-centered cubic structure Fe that crystallite dimension is 60nm
50co
50solid solution alloy powder.
Embodiment 4: crystallite dimension is the body-centered cubic structure Fe of 80nm
70co
30the preparation of solid solution alloy powder
Nine water ferric nitrates, cobalt nitrate hexahydrate, glycine and EDTA are dissolved in deionized water by a certain percentage, wiring solution-forming, heated solution is to vigorous oxidation reduction reaction occurs, obtain Nanoscale Iron cobalt/cobalt oxide precursor powder, wherein the mol ratio of cobalt nitrate hexahydrate and nine water ferric nitrates is 0.41:1, the mol ratio of glycine and nine water ferric nitrates is the mol ratio of 1:1, EDTA and nine water ferric nitrates is 1:1; By precursor powder reductase 12 hour in hydrogen atmosphere at 800 DEG C, obtain the body-centered cubic structure Fe that crystallite dimension is 80nm
70co
30solid solution alloy powder.
Embodiment 5: crystallite dimension is the body-centered cubic structure Fe of 50nm
70co
30the preparation of solid solution alloy powder
Nine water ferric nitrates, cobalt nitrate hexahydrate, glycine and glucose are dissolved in deionized water by a certain percentage, wiring solution-forming, heated solution is to vigorous oxidation reduction reaction occurs, obtain Nanoscale Iron cobalt/cobalt oxide precursor powder, wherein the mol ratio of cobalt nitrate hexahydrate and nine water ferric nitrates is 0.41:1, the mol ratio of glycine and nine water ferric nitrates is 0.5:1, and the mol ratio of glucose and nine water ferric nitrates is 1:1; By precursor powder reductase 12 hour in hydrogen atmosphere at 600 DEG C, obtain the body-centered cubic structure Fe that crystallite dimension is 50nm
70co
30solid solution alloy powder.
Claims (2)
1. there is a preparation method for body-centered cubic structure Nanoscale Iron cobalt solid solution alloy powder, it is characterized in that comprising the steps:
1) solwution method prepares nano-oxide precursor powder: ferric nitrate, cobalt nitrate, reducing agent and complexing agent are dissolved in deionized water by a certain percentage, wiring solution-forming, heated solution, until there is vigorous oxidation reduction reaction, obtains Nanoscale Iron cobalt/cobalt oxide precursor powder;
2) reducing: by step 1) precursor powder that obtains reduces in hydrogen or cracked ammonium atmosphere, and reduction temperature is 300 ~ 900 DEG C, and the recovery time is 1 ~ 3 hour, obtains the Nanoscale Iron cobalt solid solution alloy powder with body-centered cubic structure.
2. a kind of preparation method with body-centered cubic structure Nanoscale Iron cobalt solid solution alloy powder according to claim 1, it is characterized in that step 1) in reducing agent be at least one in urea, glycine, the mol ratio of reducing agent and ferric nitrate is (0.05 ~ 3): 1; Complexing agent is at least one in glucose, citric acid and tetraacethyl diaminoethanes (EDTA), and the mol ratio of complexing agent and ferric nitrate is (0.5 ~ 1.5): 1; In target Nanoscale Iron cobalt alloy powder, the ratio of iron cobalt is determined by the ratio of ferric nitrate in raw material and cobalt nitrate, ensures the mass fraction 30 ~ 70% of iron in target Nanoscale Iron cobalt alloy powder, the mass fraction 70 ~ 30% of cobalt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510338295.8A CN104874807A (en) | 2015-06-17 | 2015-06-17 | Preparation method for nanometer iron-cobalt solid solution alloy powder with body-centered cubic structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510338295.8A CN104874807A (en) | 2015-06-17 | 2015-06-17 | Preparation method for nanometer iron-cobalt solid solution alloy powder with body-centered cubic structure |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104874807A true CN104874807A (en) | 2015-09-02 |
Family
ID=53942628
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510338295.8A Pending CN104874807A (en) | 2015-06-17 | 2015-06-17 | Preparation method for nanometer iron-cobalt solid solution alloy powder with body-centered cubic structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104874807A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108555314A (en) * | 2018-07-12 | 2018-09-21 | 青岛大学 | A kind of high magnetic loss, wideband FeCo electromagnetic-wave absorbents and preparation method thereof |
| CN114433860A (en) * | 2021-12-22 | 2022-05-06 | 复旦大学 | Micron-scale succulent porous iron-cobalt alloy and preparation and application thereof |
| CN115415522A (en) * | 2022-09-30 | 2022-12-02 | 复旦大学 | Multi-shell porous iron-cobalt alloy and preparation method and application thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06163230A (en) * | 1992-11-26 | 1994-06-10 | Kanegafuchi Chem Ind Co Ltd | Method of manufacturing magnetic powder for bonded magnet |
| CN1301205A (en) * | 1998-05-20 | 2001-06-27 | H·C·施塔克公司 | Sinter-active metal and alloy powders for powder metallurgy applications and methods for their production and their use |
| CN1371774A (en) * | 2001-02-28 | 2002-10-02 | 李�杰 | Method for preparing nano metal composite particle |
| CN1454851A (en) * | 2002-04-17 | 2003-11-12 | 国际商业机器公司 | Synthesizing of magnetite nano particles and method for forming iron-base nano material |
| CN1947998A (en) * | 2005-10-14 | 2007-04-18 | 陈福生 | Multi-layered material having stereo-texture |
| CN101299914A (en) * | 2008-06-20 | 2008-11-05 | 广东工业大学 | Nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof |
| CN101956119A (en) * | 2010-09-19 | 2011-01-26 | 北京科技大学 | Preparation method of prealloying powder for dispersion strengthening metal by low-temperature combustion synthesis method |
| JP2013185222A (en) * | 2012-03-08 | 2013-09-19 | Japan Science & Technology Agency | bcc TYPE FeCo ALLOY PARTICLE AND MANUFACTURING METHOD THEREOF, AND MAGNET |
-
2015
- 2015-06-17 CN CN201510338295.8A patent/CN104874807A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06163230A (en) * | 1992-11-26 | 1994-06-10 | Kanegafuchi Chem Ind Co Ltd | Method of manufacturing magnetic powder for bonded magnet |
| CN1301205A (en) * | 1998-05-20 | 2001-06-27 | H·C·施塔克公司 | Sinter-active metal and alloy powders for powder metallurgy applications and methods for their production and their use |
| CN1371774A (en) * | 2001-02-28 | 2002-10-02 | 李�杰 | Method for preparing nano metal composite particle |
| CN1454851A (en) * | 2002-04-17 | 2003-11-12 | 国际商业机器公司 | Synthesizing of magnetite nano particles and method for forming iron-base nano material |
| CN1947998A (en) * | 2005-10-14 | 2007-04-18 | 陈福生 | Multi-layered material having stereo-texture |
| CN101299914A (en) * | 2008-06-20 | 2008-11-05 | 广东工业大学 | Nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof |
| CN101956119A (en) * | 2010-09-19 | 2011-01-26 | 北京科技大学 | Preparation method of prealloying powder for dispersion strengthening metal by low-temperature combustion synthesis method |
| JP2013185222A (en) * | 2012-03-08 | 2013-09-19 | Japan Science & Technology Agency | bcc TYPE FeCo ALLOY PARTICLE AND MANUFACTURING METHOD THEREOF, AND MAGNET |
Non-Patent Citations (2)
| Title |
|---|
| 吴子秋等: "纳米晶Fe-Ni和Fe-Co粉的微波磁性能", 《宇航材料工艺》 * |
| 李伟等: "机械研磨处理纳米晶FeCo合金结构的TEM研究", 《电子显微学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108555314A (en) * | 2018-07-12 | 2018-09-21 | 青岛大学 | A kind of high magnetic loss, wideband FeCo electromagnetic-wave absorbents and preparation method thereof |
| CN114433860A (en) * | 2021-12-22 | 2022-05-06 | 复旦大学 | Micron-scale succulent porous iron-cobalt alloy and preparation and application thereof |
| CN115415522A (en) * | 2022-09-30 | 2022-12-02 | 复旦大学 | Multi-shell porous iron-cobalt alloy and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103157803B (en) | A kind of solid state reaction prepares the method for Nanoalloy | |
| Gandha et al. | High energy product developed from cobalt nanowires | |
| CN101299914B (en) | Nanocrystalline ultra-fine alloy powder electromagnetic wave absorbent and preparation method thereof | |
| CN104439269B (en) | The synthesis and annealing of manganese bismuth nanoparticle | |
| CN100369703C (en) | Fe nanowire and preparation method thereof | |
| CN101817088B (en) | Preparation method of Pt-Ni alloy nano particle and colloidal dispersion system thereof | |
| CN102601384B (en) | Chemical method for preparing cobalt nickel nanoscale alloy powder | |
| CN103170636A (en) | Method for preparing nano metal simple substance through solid-state chemical reaction | |
| CN103447549B (en) | Preparation method of cobalt nanosphere | |
| CN100374231C (en) | Preparation method of nano-cobalt powder | |
| CN104439280A (en) | Simultaneous preparing method of cobalt hydroxide and cobalt powder | |
| CN104874807A (en) | Preparation method for nanometer iron-cobalt solid solution alloy powder with body-centered cubic structure | |
| CN103170635A (en) | Method for preparing spherical molybdenum powder | |
| CN104985194B (en) | A kind of preparation method at oxide dispersion intensifying iron cobalt nano composite powder end | |
| CN105033277A (en) | Preparation technology of superfine spherical nickel, cobalt and iron ternary alloy powder | |
| CN104525962A (en) | Method for preparing nanoscale oxide dispersion strengthening iron-based composite powder | |
| CN103524125A (en) | Process method for preparing carbon-black-loaded cobalt zinc ferrite wave-absorbing material | |
| CN104909412A (en) | Preparation method of magnetic Fe2O3/Fe3O4 nano-heteroplasmon particles | |
| CN104551004B (en) | The chemical preparation process of a kind of ferro-cobalt Nanoalloy powder body | |
| CN105290419A (en) | Fishbone-shaped core-shell structure nanometer nickel-copper alloy powder and preparation method thereof | |
| CN109604625B (en) | Method for preparing platinum-based binary alloy nanoparticles by using transition metal oxide and platinum metal nanoparticles as precursors | |
| CN104889415A (en) | Preparation method of nano nickel powder | |
| CN104525967A (en) | Nanoscale iron powder preparation method | |
| CN108373327B (en) | Nickel-zinc-cerium ferrite soft magnetic material and preparation method thereof | |
| CN103722176A (en) | Method for doping rare earth lanthanum in nano molybdenum powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150902 |