CN101220447A - Method for producing Fe-B amorphous alloy nano-wire - Google Patents
Method for producing Fe-B amorphous alloy nano-wire Download PDFInfo
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- CN101220447A CN101220447A CN 200810052093 CN200810052093A CN101220447A CN 101220447 A CN101220447 A CN 101220447A CN 200810052093 CN200810052093 CN 200810052093 CN 200810052093 A CN200810052093 A CN 200810052093A CN 101220447 A CN101220447 A CN 101220447A
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Abstract
The invention aims at providing a method for preparing magnetic Fe-B amorphous alloy nanometer lines and is characterized in that Fe-B amorphous alloy is prepared in an electromagnetic field device by chemical reduction; a reactor is placed in the electromagnetic field device and divalent ferric salt with certain concentration is reduced with reducing agents; direct current or alternating current is pumped into coils of the electromagnetic field to generate respectively constant magnetic fields or alternating magnetic fields; Fe-B amorphous alloys with different shapes and linear structures can be obtained by making reducing reaction in different magnetic fields; known from the measurement, Fe-B amorphous alloy nanometer lines with different shapes are provided with different magnetic properties. The reaction has the advantages that the reaction is carried out at a normal temperature, and the conditions are simple, practical, and easy to control; thus the invention can meet the requirements of actual production.
Description
Technical field
The present invention relates to a kind of method for preparing amorphous alloy nano-wire, a kind of method for preparing magnetic Fe-B amorphous alloy nano-wire in magnetic field of saying so more specifically.
Background technology
The application of magnetic Nano material is to relate to every field.At machinery, electricity, optics, magnetics, the chemistry and biology field has a wide range of applications.The characteristic of magnetic Nano material is different from conventional magneticsubstance, and its reason is that the feature physical length that is associated with magnetic dependence is in nanometer scale just.For example: magnetic single domain size, superparamagnetism critical size, exchange interaction length, and electronics mean free path etc. roughly is in the 1-100nm magnitude.When the size of magnetic substance is suitable with these feature physical length, will present special magnetic property.
Nano-magnetic transition metal material and oxide compound thereof, the nano transition metal material that particularly has shape anisotropy, because its excellent character and at high density magnetic recording, magnetic sensing, the application potential in fields such as absorbing material and catalysis and be subjected to extensive concern.In recent years, the investigator has found the method for many synthesis of nano transition metal materials and oxide compound thereof, as microemulsion method, hydrothermal synthesis method, and borohydride reduction method and template synthesis method etc.
Because magnetic field can influence growth and the assembling that is in magnetic particle wherein, therefore in preparation process, introduce the pattern that magnetic field can change obtained nanoparticle effectively.In recent years, magnetic field is applied to synthesizing and chemical vapour deposition reaction as electrochemical reaction, solid state reaction, hydro-thermal, particularly among the preparation feedback of nano material among the number of chemical reaction as a kind of common means.So far, many research groups all carried out relevant research to this field.Sun etc. are at hydrazine hydrate reduction NiCl
2With introduced intensity in the reaction of PVP mixed system and be respectively 0.1T, the stationary magnetic field of 0.25T and 0.4T has prepared one dimension Ni nano wire (Sun, the L.X. of linearity; Chen, Q.W.; Tang, Y.; Xiong, Y.; Chem.Comm.2007,27:2844).Wang etc. are at hydrazine hydrate reduction FeCl
2Reaction in introduced intensity and be respectively 0.1T, the magnetic field of 0.25T and 0.35T has prepared Fe
3O
4Wire monocrystalline (Wang, J.; Chen, Q.W.; Zeng, C.; Hou, B.Y.; Adv.Mater.2004,16:137).Niu etc. prepare the externally-applied magnetic field of having introduced 0.25T in the process of nanometer Ni adding PEG and CTAB, have realized the self-assembly of needle-like Ni, and have formed nanometer Ni (Niu, the H.L. with one-dimentional structure; Chen, Q.W.; Ning, M.; Jia, Y.S.; Wang, X.J.; J.Phys.Chem.B 2004,108:3996).This shows that investigating externally-applied magnetic field is a job highly significant for the self-assembly of magneticsubstance and the influence of process of growth.But some present experimental techniques concentrate on the synthetic or solvent thermal synthetic method of hydro-thermal of using mostly, and the temperature and pressure that reaction needed is higher could generate the nanoparticle of transition metal.And, in reaction, need to introduce externally-applied magnetic field with higher-strength, just can synthesize nano material with one dimension linear structure.So this method may and not be suitable for the large-scale commercial production of one dimension wire nano material.
Summary of the invention
The present invention has introduced a kind of by introducing the electromagnetic field that adds of dissimilar and intensity, uses KBH
4The method for preparing one dimension Fe-B amorphous alloy nano-wire for reductive agent.The externally-applied magnetic field that applies in the reaction plays important effect in the formation of wire Fe-B amorphous alloy, and is not compared with introducing the magnetic field products therefrom by the product that this method obtains, and variation has also taken place its magnetic property.
Characteristics of the present invention are to have prepared a kind of diameter in 50～80 nanometers, the Fe-B amorphous alloy nano-wire of length about 1～15 micron, product size uniformity.This method is simple, can easyly prepare one dimension Fe-B amorphous alloy nano-wire apace.
The preparation process of Fe-B amorphous alloy nano-wire is as follows:
Step 1, employing solubility divalent iron salt are raw material, are mixed with solution with deionized water dissolving, and the content of iron ion is 0.01～0.5mol/L in the solution.
Step 2, add complexing agent in the solution of step 1 gained, its add-on is 10～100g/L.
Step 3, add tensio-active agent in the solution of step 1 gained, its add-on is 2～15g/L.
Step 4, add complexing agent and tensio-active agent in the solution of step 1 gained, it is identical that its add-on such as step 2, step 3 provide.
Step 5, with step 1, or step 2, or step 3, or the solution of step 4 gained feeds argon gas and removes the oxygen that is dissolved in wherein;
Step 6, with KBH
4Be dissolved in the deionized water, be mixed with the solution that concentration is 0.01～0.5mol/L.
Step 7, the solution of step 6 gained is under agitation joined in the solution of step 5 gained, rate of addition is 1～5ml/min.All the time feed argon gas in the reaction, and keep temperature of reaction at 25 ℃, the reaction times is 30～120min.In the reaction process, reaction vessel is placed electromagnetic field device, feed direct current or alternating current at the electromagnetic field coil, by regulating alive size, the magneticstrength that the controlling magnetic field device produces is 0～0.20T.
Described solubility divalent iron salt is an iron protochloride, ferrous sulfate or ferrous ammonium sulphate, preferred iron protochloride.
Described complexing agent is tartrate, sodium tartrate, Seignette salt, citric acid, Trisodium Citrate or edetate, preferred sodium tartrate.
Described tensio-active agent is a polyvinylpyrrolidone, cetyl trimethylammonium bromide, sodium laurylsulfonate or polyoxyethylene glycol, preferably polyethylene pyrrolidone.
Description of drawings
The SEM photo (* 20000) of the Fe-B amorphous alloy nano-wire that Fig. 1 prepares in direct magnetic field
The SEM photo (* 15000) of the Fe-B amorphous alloy nano-wire that Fig. 2 prepares in AC magnetic field
Fig. 3 introduces the SEM photo (* 20000) of the Fe-B amorphous alloy nano-wire of PVP preparation in direct magnetic field
Embodiment
Embodiment 1
The employing iron protochloride is a raw material, is mixed with solution with deionized water dissolving, and the concentration of iron ion is 0.05mol/L in the solution, and solution feeds argon gas and removes the oxygen that is dissolved in wherein.With KBH
4Be dissolved in the deionized water, be mixed with the solution that concentration is 0.1mol/L.KBH
4Solution under agitation joins in the solution of ferrous chloride, and rate of addition is 1ml/min.All the time feed argon gas in the reaction, and keep temperature of reaction at 25 ℃, the reaction times is 45min.In the reaction process, reaction vessel is placed electromagnetic field device, feed galvanic current in the electromagnetic field coil, by regulating alive size, the magneticstrength that the controlling magnetic field device produces is 0.06T.Make Fe-B amorphous alloy nano-wire A, its SEM photo is seen accompanying drawing 1.As seen from the figure, the diameter of gained Fe-B amorphous alloy nano-wire is about 50～60 nanometers, and length is 3～5 microns.
Embodiment 2～3
The preparation method of Fe-B amorphous alloy nano-wire such as embodiment 1, the magneticstrength that controlling magnetic field device among the embodiment 1 is produced changes 0.03T or 0T into, and all the other conditions make Fe-B amorphous alloy nano-wire B, C with embodiment 1.
Embodiment 4
The preparation method of Fe-B amorphous alloy nano-wire such as embodiment 1 change the electric current that feeds among the embodiment 1 into alternating-current, and the magneticstrength that the controlling magnetic field device produces changes 0.02T into, and all the other conditions make Fe-B amorphous alloy nano-wire D with embodiment 1.
Embodiment 5～6
The preparation method of Fe-B amorphous alloy nano-wire such as embodiment 4, the magneticstrength that embodiment 4 controlling magnetic field devices are produced changes 0.04T or 0.06T into, and all the other conditions make Fe-B amorphous alloy nano-wire E, F with embodiment 4.The SEM photo of F is seen accompanying drawing 2, and as seen from the figure, the diameter of gained Fe-B amorphous alloy nano-wire is 50～60 nanometers, and length is 5～8 microns.
Embodiment 7～9
The preparation method of Fe-B amorphous alloy nano-wire such as embodiment 1 change into 0.01g/L with solution of ferrous chloride concentration among the embodiment 1,0.10g/L, and 0.50g/L, all the other conditions make Fe-B amorphous alloy nano-wire G～I with embodiment 1.
Embodiment 10～12
The preparation method of Fe-B amorphous alloy nano-wire such as embodiment 1 are with KBH among the embodiment 1
4Strength of solution is changed into 0.01g/L, 0.25g/L, and 0.50g/L, all the other conditions make Fe-B amorphous alloy nano-wire J～L with embodiment 1.
Embodiment 13～14
The preparation method of Fe-B amorphous alloy nano-wire such as embodiment 1 are with KBH among the embodiment 1
4The rate of addition of solution is changed into 3ml/min or 5ml/min or all the other conditions with embodiment 1, makes Fe-B amorphous alloy nano-wire M and N.
Embodiment 15～17
The preparation method of Fe-B amorphous alloy nano-wire such as embodiment 1 change into 30min with the reaction times among the embodiment 1,60min, and all the other conditions of 90min make Fe-B amorphous alloy nano-wire O～Q with embodiment 1.
Embodiment 18～21
The preparation method of Fe-B amorphous alloy nano-wire such as embodiment 1 will add sodium tartrate 10g/L in the solution of ferrous chloride among the embodiment 1,23g/L, and 46g/L, 100g/L, all the other conditions make Fe-B amorphous alloy nano-wire R～U with embodiment 1.
Embodiment 22～24
The preparation method of Fe-B amorphous alloy nano-wire such as embodiment 1 will add polyvinylpyrrolidone 2g/L in the solution of ferrous chloride among the embodiment 1,10g/L, and 15g/L, all the other conditions make Fe-B amorphous alloy nano-wire V～X with embodiment 1.
Embodiment 25
The preparation method of Fe-B amorphous alloy nano-wire such as embodiment 1 will add sodium tartrate 2.3g and polyvinylpyrrolidone 1g in the solution of ferrous chloride among the embodiment 1, all the other conditions make Fe-B amorphous alloy nano-wire Y with embodiment 1.Its SEM photo is seen accompanying drawing 3.As seen from the figure, this the diameter of Fe-B amorphous alloy nano-wire about 80 nanometers, length is at 10～15 microns.
Embodiment 26
Use vibrating sample magnetometer to measure the magnetic property of gained sample, the associated magnetic mathematic(al) parameter of part Fe-B amorphous alloy nano-wire is as shown in table 1.By the data of table 1 as can be known, the noticeable change along with the variation of the externally-applied magnetic field of introducing in the preparation of the magnetics parameter of sample: coercive force increases gradually, and saturation induction intensity reduces; That is to say easier magnetization the when sample is in the magnetic field, and after removing magnetic field, can be good at keeping magnetic.Therefore the Fe-B amorphous alloy nano-wire of preparation may well be used in magnetic recording material or magnetic catalyst matrix in this way.
The associated magnetic mathematic(al) parameter of table 1 gained Fe-B amorphous alloy nano-wire
| Sample | Saturation induction density (B s) (emu/g) | Remanent magnetism (B r) (emu/g) | Coercive force (H c) (Oe) |
| A | 98.51 | 30.87 | 361.2 |
| B | 100.5 | 30.44 | 352.0 |
| C | 121.0 | 17.51 | 192.8 |
Claims (8)
1. the present invention has introduced a kind of by introducing the electromagnetic field that adds of dissimilar and intensity, use KBH
4The method for preparing one dimension Fe-B amorphous alloy nano-wire for reductive agent.The externally-applied magnetic field that applies in the reaction plays important effect in the formation of wire Fe-B amorphous alloy, and is not compared with introducing the magnetic field products therefrom by the product that this method obtains, and variation has also taken place its magnetic property.
Characteristics of the present invention are to have prepared a kind of diameter in 50～80 nanometers, the Fe-B amorphous alloy nano-wire of length about 1～15 micron, product size uniformity.This method is simple, can easyly prepare one dimension Fe-B amorphous alloy nano-wire apace.
The preparation of catalytic reduction dechlorinating agent:
Reaction vessel is placed electromagnetic field device, in the electromagnetic field coil, feed direct current or alternating current, by regulating alive size, the magnetic field of the varying strength that the controlling magnetic field device produces.With the divalent iron salt is raw material, is dissolved in deionized water and is mixed with solution, and the concentration of iron ion is 0.01～0.5mol/L in the solution, and solution feeds argon gas and is dissolved in wherein oxygen with removal.With KBH
4Be dissolved in the deionized water, be mixed with the solution that concentration is 0.01～0.5mol/L.KBH
4Solution under agitation joins in the ferrous iron solution, and rate of addition is 0.2～5ml/min.All the time feed argon gas in the reaction, and keep temperature of reaction at 0～60 ℃, the reaction times is 15～120min.The product of gained is separated, and successively with deionized water and absolute ethanol washing.Product after the washing is dry 2h in vacuum drier, and temperature is 60 ℃.Can add an amount of complexing agent and tensio-active agent in the reaction.
2. be to feed direct current stationary magnetic field that produces and the alternating magnetic field that feeds the alternating current generation according to the described magnetic field of claim 1 at the electromagnetic field coil.
3. the concentration according to iron ion in the described solution of claim 1 is 0.01～0.5mol/L, and preferred concentration is 0.05mol/L.
4. according to adding KBH in the described reaction of claim 1
4Strength of solution is 0.01～0.5mol/L, preferred 0.1mol/L.
5. according to the described KBH of claim 1
4The drips of solution acceleration is 0.2～5ml/min, preferred 1ml/min.
6. be 0～60 ℃ according to the described temperature of reaction of claim 1, preferred 25 ℃.
7. be 15～120min according to the described reaction times of claim 1, preferred 45min.
8. according to the described tensio-active agent of claim 1 and complexing agent preferably polyethylene pyrrolidone and sodium tartrate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086025A (en) * | 2011-01-07 | 2011-06-08 | 中国科学技术大学 | Preparation method of one-dimensional (1D) flexible nano-material assembly body |
| CN104014815A (en) * | 2014-06-19 | 2014-09-03 | 厦门大学 | Cobalt-based amorphous nanometer wave-absorbing material and synthetic method of cobalt-based amorphous nanometer wave-absorbing material |
| CN105107506A (en) * | 2015-07-24 | 2015-12-02 | 山西大学 | Preparation method for modified activated carbon used for catalysis of hydrogen peroxide oxidation |
| CN110625137A (en) * | 2019-10-16 | 2019-12-31 | 重庆邮电大学 | Preparation method of monodisperse iron nanowire with controllable structure and product |
| CN115323250A (en) * | 2022-08-19 | 2022-11-11 | 安徽中环软磁科技有限公司 | Process for preparing amorphous nanocrystalline magnetic material |
-
2008
- 2008-01-17 CN CN 200810052093 patent/CN101220447B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086025A (en) * | 2011-01-07 | 2011-06-08 | 中国科学技术大学 | Preparation method of one-dimensional (1D) flexible nano-material assembly body |
| CN104014815A (en) * | 2014-06-19 | 2014-09-03 | 厦门大学 | Cobalt-based amorphous nanometer wave-absorbing material and synthetic method of cobalt-based amorphous nanometer wave-absorbing material |
| CN105107506A (en) * | 2015-07-24 | 2015-12-02 | 山西大学 | Preparation method for modified activated carbon used for catalysis of hydrogen peroxide oxidation |
| CN110625137A (en) * | 2019-10-16 | 2019-12-31 | 重庆邮电大学 | Preparation method of monodisperse iron nanowire with controllable structure and product |
| CN115323250A (en) * | 2022-08-19 | 2022-11-11 | 安徽中环软磁科技有限公司 | Process for preparing amorphous nanocrystalline magnetic material |
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