CN108941611A - A kind of preparation method and product of ferromagnetic nano wire - Google Patents

A kind of preparation method and product of ferromagnetic nano wire Download PDF

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CN108941611A
CN108941611A CN201811094904.XA CN201811094904A CN108941611A CN 108941611 A CN108941611 A CN 108941611A CN 201811094904 A CN201811094904 A CN 201811094904A CN 108941611 A CN108941611 A CN 108941611A
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solution
ferromagnetic
nano wire
salt
sodium
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CN108941611B (en
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杨平安
李锐
刘琳
卢毅
李欣晏
孙杨
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Chongqing Tianyu New Material Technology Research Institute Co ltd
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Chongqing University of Post and Telecommunications
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/07Metallic powder characterised by particles having a nanoscale microstructure
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B22F2009/245Reduction reaction in an Ionic Liquid [IL]

Abstract

The present invention relates to a kind of preparation method of ferromagnetic nano wire and products, belong to technical field of nano material, ferromagnetic metal mixed salt solution is prepared by raw material of ferromagnetic metal salt, stabilizer, complexing agent and surfactant first in this method, then reducing agent solution is injected by way of injection, after reacted, solid product is made, it is the solid product is cleaned, dry.This method synthetic route is simple, technique is controllable, normal temperature and pressure reaction, meets needs of production, is suitble to industrialized production, while can overcome traditional local reduction way that can only prepare the defect of the certain ferromagnetic nano wire of draw ratio.Ferromagnetic nano wire obtained has good orientation in this way, and for diameter in 100nm hereinafter, length is at 3~10 μm, draw ratio is high, has good flexibility, magnetic property and microwave absorbing property.

Description

A kind of preparation method and product of ferromagnetic nano wire
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of preparation method and product of ferromagnetic nano wire.
Background technique
Ferromagnetic nano wire is Nano grade (E-9M) iron atom stacks 1-dimention nano made of growth according to a certain direction Material.Nanoscale size and unique structure, so that ferromagnetic nano wire shows unique object that many body phase materials do not have Effect is managed, mainly includes small-size effect, surface-interface effect, quantum size effect and macro quanta tunnel effect etc..Solely The characteristics such as special structure and peculiar light, electricity, magnetic make ferromagnetic nano wire in social each field of industry using increasingly extensive. For example, big saturation magnetization, high coercivity, good inoxidizability, high signal-to-noise ratio, so that being with ferromagnetic nano wire The performance of tape and the soft or hard disk of large capacity can be substantially improved in the high-performance magnetism recording materials on basis;Ferromagnetic nano wire has not It is same as the mechanism of conventional material, the absorbent properties excellent to electromagnetic wave are shown in wideband segment limit, are widely applied The compound and Structural Stealth Materials such as the electromagnetic wave stealth material of microwave frequency band, visible light-infrared light stealth material in military affairs, with And screening material against electromagnetic radiation;It is the directed agents of carrier based on ferromagnetic nano wire, can use the soft magnetic characteristic of ferromagnetic nano wire, High concentration medicine is gathered in lesions position under the action of an external magnetic field, to carry out specific aim targeted therapy to pathogenic site; Using ferromagnetic nano wire as the ferrofluid of magnetic-particle, there is good resistance to settling and shear yield stress, in vibration damping, close Envelope, polishing, sound adjusting, medical instrument, light show etc. that fields show huge application potential;In addition, ferromagnetic nano wire is also It is widely used in the catalyst of silicon nanowires and carbon nano-fiber growth.It the excellent performance of ferromagnetic nano wire and is widely applied, makes It becomes one of the research hotspot in material science and Condensed Matter Physics.
Template synthesis method, lithographic printing and metallizing by evaporation are three kinds of common methods for preparing ferromagnetic nano wire.It is logical Cross template and prepare ferromagnetic nano wire, be with nano grade pore film in react so that generate ferromagnetic particle along hole without leave Assembling forms nano wire, uses highly corrosive agents then to remove the film as template, this process is inevitably received to ferromagnetic The purity of rice noodles has an impact, while certain harm can be also caused to environment;Lithographic printing utilizes additional directional magnetic field, Ferromagnetic particle on matrix is self-assembled into regular nano wire, this process is related to the selection of matrix, magnetic field parameter, and produces Measure it is low so that preparation cost is higher;And metallizing by evaporation evaporates formation using ferromagnetic metallic granular system or silk at high temperature Ferromagnetic particle solidifies on matrix is assembled into nano wire, such as Chinese patent CN200410088423.X discloses one kind in silicon substrate The method that monocrystalline iron nanometer thread is grown on body, by connecing on the electrode spiral helicine iron wire, and passes to 20~35 amperes of electricity Stream is heated, evaporation iron wire deposited on silicon substrate, there are complicated for operation, low output, it is at high cost the defects of.It is above-mentioned to overcome The defect of method, emerges some new methods for preparing ferromagnetic nano wire, and Chinese patent CN200710056737.5 discloses one The preparation method of kind ferromagnetic nano wire, passes through and sodium hydroxide or ammonium hydroxide is added in iron nitrate solution, is made Fe (OH)3, then Fe (OH) is obtained than mixing and ball milling by certain mass with sodium chloride3After/NaCl composite powder, restored at a certain temperature with hydrogen Fe/NaCl is obtained, is cleaned by ultrasonic eventually by deionized water and obtains Fe nanowire.This method operating procedure is more complicated, and It is related to the more demanding professional equipment such as ball milling and hydrogen reducing.Chinese patent CN200610018655.7 and Chinese science technology Wanquan Jiang of university et al. (Jiang W Q et al., J.Magn.Magn.Mater., 323 (2011) 3246- 3250) local reduction way is utilized, using soluble ferrous iron or trivalent iron salt as raw material, it is molten to be dissolved in distilled water obtained molysite Liquid, and reducing agent solution is added dropwise in iron salt solutions and is reacted, is filtered, drying prepares Fe nanowire.Whole process is at normal temperature It carries out, synthetic route is simple, however dropwise addition process is slower, and the Fe nanowire draw ratio prepared is limited.
Therefore, it is badly in need of that a kind of process is simple, speed is fast, makes the ferromagnetic nano wire finally prepared purity is high, good dispersion, big Small preparation method uniform, length is controllable.
Summary of the invention
In view of this, one of the objects of the present invention is to provide a kind of preparation methods of ferromagnetic nano wire;The second purpose exists In providing a kind of ferromagnetic nano wire.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, a kind of preparation method of ferromagnetic nano wire, described method includes following steps:
(1) ferromagnetic metal salt is soluble in water, then adjust pH value be 10~12, add stabilizer, complexing agent and Surfactant after stirring, removes the oxygen in solution, forms ferromagnetic metal mixed salt solution;The ferromagnetic metal salt Ferromagnetic metal salinity is 0.05~0.15mol/L in mixed solution, and stabilizer concentration is 0.02~0.04mol/L, complexing Agent concentration is 0.001~0.002mol/L, and surfactant concentration is 0.002~0.003mol/L;
(2) after dissolving reduce agent in solution, reducing agent solution is formed;Reductant concentration is 0.9 in the reducing agent solution ~2mol/L;
(3) reducing agent solution formed in step (2) is entered step to the ferromagnetism formed in (1) by way of injection In metal mixed salt solution, after the completion of reducing agent solution injection, 30~45min is reacted at 20~40 DEG C, consolidate Body product, it is the solid product is cleaned, dry.
Preferably, in step (1), the ferromagnetic metal salt is one of molysite, nickel salt or cobalt salt.
Preferably, the molysite is ferrous sulfate heptahydrate, frerrous chloride, ferric sulfate, iron chloride, ferric nitrate, ironic citrate At least one of;The nickel salt is at least one of nickel sulfate hexahydrate, nickel chloride, nickel nitrate, nickel acetate;The cobalt salt is At least one of cobalt chloride, cobaltous sulfate, cobalt nitrate, cobalt acetate.
Preferably, in step (1), when adjusting pH value PH regulator used be sodium hydroxide, sodium bicarbonate, sodium carbonate, At least one of lime.
Preferably, in step (1), the stabilizer be dodecyl vinegar propylhomoserin, gelatin, cysteine, diiodotyrosine, At least one of cystine, dimethyl disulfide carbamate;The complexing agent is polyvinylpyrrolidone, glycerol, ethylenediamine Tetraacetate, sodium ammonium triacetate, sodium pyrophosphate, ethylenediamine tetraacetic methene sodium phosphate, potassium pyrophosphate, diethylenetriamine pentacarboxylic acid salt, At least one of ammonium chloride;The surfactant is polystyrene, polyethylene glycol, sulfamic acid sodium, detergent alkylate sulphur At least one of sour sodium, 1,4 butynediols, sulfamic acid potassium, Cetrimide.
Preferably, in step (2), the reducing agent is sodium borohydride, potassium borohydride, aluminium borohydride, hydrazine hydrate, sulfuric acid At least one of hydrazine, formaldehyde or dimethylamino borine.
Preferably, in step (2), the solution is one of water, dehydrated alcohol or aqueous solution of ethyl alcohol.
Preferably, in step (3), the cleaning is specially to be in the pH value that water and dehydrated alcohol are alternately cleaned to cleaning solution It is neutral;The drying is specially dry 7~9h in 50~70 DEG C under nitrogen protection.
Preferably, in step (2), the speed of the injection is 50~90mL/s.
2, the ferromagnetic nano wire prepared by the method.
The beneficial effects of the present invention are: the present invention provides a kind of preparation method of ferromagnetic nano wire and product, the party Method synthetic route is simple, technique is controllable, normal temperature and pressure reaction, meets needs of production, is suitble to industrialized production, while can Overcome traditional local reduction way that can only prepare the defect of the certain ferromagnetic nano wire of draw ratio.The reducing agent solution of excessive concentrations with When ferromagnetic metal salt meets, ferromagnetic ion, which can be reduced, generates feeromagnetic metal core, and generates a large amount of bubble, adopts in the present invention Reducing agent solution high speed injection is entered into ferromagnetic metal salting liquid with injection system, the two contact is very unexpected, can generate play Strong reaction generates feeromagnetic metal core and bubble, and the feeromagnetic metal core formed can combine with bubble and form community to reduce Surface energy.Meanwhile nanoscale feeromagnetic metal nuclear energy reaches self assembly, i.e. feeromagnetic metal core holds during synthesis is with growth Easily spontaneous or induction is assembled into the micro-nano granules with special appearance.The Crack cause of nano wire pattern exists in the present invention In the reducing agent for injecting entrance can immediately restore the feeromagnetic metal ion generation feeromagnetic metal core of surrounding, and these ferromagnetic gold Belong to core convergence collection and is combined into nanosphere.Since the reducing agent that injection enters is in the form of a column stream in reaction solution, it is reduced The feeromagnetic metal core of generation is also to be in the form of a column distribution, and with the life of nanometer spherical particle during mutual aggregation combines Long, the ball particle closed on can be connected with each other under the deposition layer by layer of feeromagnetic metal core, combine together, finally along injection The nano wire of columnar flow formation high length-diameter ratio.Ferromagnetic nano wire obtained has good orientation in this way, and diameter is in 100nm Hereinafter, length is at 3~10 μm, draw ratio is high, has good flexibility, magnetic property and microwave absorbing property.
Detailed description of the invention
In order to keep the purpose of the present invention, technical scheme and beneficial effects clearer, the present invention provides following attached drawing and carries out Illustrate:
Fig. 1 is the SEM figure of the ferromagnetic nano wire for preparing under 1.75 ten thousand times in embodiment 1;
Fig. 2 is the SEM figure of the ferromagnetic nano wire for preparing under 100,000 times in embodiment 1;
Fig. 3 is the XRD diagram of the ferromagnetic nano wire prepared in embodiment 1;
Fig. 4 is the electromagnetic wave absorption curve graph of the ferromagnetic nano wire prepared in embodiment 1;
Fig. 5 is the SEM figure of the ferromagnetic nano wire for preparing under 2.79 ten thousand times in embodiment 1;
Fig. 6 is the SEM figure of the ferromagnetic nano wire for preparing under 50,000 times in embodiment 1;
Fig. 7 is that the SEM of the ferromagnetic nano wire for preparing 12.4 ten thousand under schemes in comparative example 1.
Specific embodiment
Below by a preferred embodiment of the present invention will be described in detail.
Embodiment 1
Prepare ferromagnetic nano wire
1, a kind of preparation method of ferromagnetic nano wire, described method includes following steps:
(1) ferromagnetic metal salt (ferrous sulfate heptahydrate) is dissolved in deionized water, then with PH regulator (hydroxide Sodium) adjust pH value be 11, add stabilizer (gelatin), complexing agent (polyvinylpyrrolidone) and surfactant (poly- second two Alcohol), after stirring, nitrogen is passed through to remove the oxygen in solution, forms ferrous sulfate heptahydrate mixed solution;The ferrous sulfate heptahydrate Ferrous sulfate heptahydrate concentration is 0.05mol/L, gelatin concentration 0.02mol/L, polyvinylpyrrolidoneconcentration concentration in mixed solution For 0.0015mol/L, Polyethylene glycol 0.0025mol/L;
(2) after reducing agent (sodium borohydride) being dissolved in deionized water, sodium borohydride solution is formed;In the sodium borohydride solution Sodium borohydride concentration is 1.2mol/L;
(3) syringe is used to enter step the sodium borohydride solution formed in step (2) with the speed injection of 70mL/s (1) in the ferrous sulfate heptahydrate mixed solution formed in, after the completion of sodium borohydride solution injection, 30min is reacted at 30 DEG C, The solid product that reaction generates is collected with magnet, which is alternately cleaned with water and dehydrated alcohol to the pH value of cleaning solution After being in neutrality under nitrogen protection, dry 8h is dry in 60 DEG C.
Embodiment 2
1, a kind of preparation method of ferromagnetic nano wire, described method includes following steps:
(1) ferromagnetic metal salt (iron chloride) is dissolved in deionized water, pH is then adjusted with PH regulator (sodium bicarbonate) Value is 12, adds stabilizer (dodecyl vinegar propylhomoserin), complexing agent (glycerol) and surfactant (polystyrene), is stirred Afterwards, nitrogen is passed through to remove the oxygen in solution, forms chlorination iron mixed solution;Ferric chloride concn in the chlorination iron mixed solution For 0.08mol/L, dodecyl vinegar propylhomoserin concentration is 0.04mol/L, glycerol concentration 0.001mol/L, and polystyrene concentrations are 0.002mol/L;
(2) after reducing agent (potassium borohydride) being dissolved in dehydrated alcohol, solution of potassium borohydride is formed;In the solution of potassium borohydride Potassium borohydride concentration is 0.9mol/L;
(3) syringe is used to enter step the solution of potassium borohydride formed in step (2) with the speed injection of 50mL/s (1) in the chlorination iron mixed solution formed in, after the completion of solution of potassium borohydride injection, 45min is reacted at 20 DEG C, with magnet The solid product that reaction generates is collected, which is in neutrality with the pH value that water and dehydrated alcohol are alternately cleaned to cleaning solution Afterwards under nitrogen protection, dry 9h is dry in 50 DEG C.
Embodiment 3
1, a kind of preparation method of ferromagnetic nano wire, described method includes following steps:
(1) ferromagnetic metal salt (ironic citrate) is dissolved in deionized water, pH is then adjusted with PH regulator (sodium carbonate) Value is 10, adds stabilizer (dimethyl disulfide carbamate), complexing agent (sodium ammonium triacetate) and surfactant (dodecane Base benzene sulfonic acid sodium salt), after stirring, nitrogen is passed through to remove the oxygen in solution, forms ironic citrate mixed solution;The ironic citrate Ferric Citrate concentration is 0.15mol/L in mixed solution, and dimethyl disulfide carbamate concentration is 0.02mol/L, nitrilotriacetic acid Na concn is 0.002mol/L, and neopelex concentration is 0.003mol/L;
(2) reducing agent (hydrazine hydrate) is dissolved in dehydrated alcohol and the deionized water ethyl alcohol that 1:1 is mixed to form by volume After aqueous solution, hydrazine hydrate solution is formed;Concentration of hydrazine hydrate is 2mol/L in the hydrazine hydrate solution;
(3) use syringe that the hydrazine hydrate solution formed in step (2) is entered step (1) with the speed injection of 60mL/s In the ironic citrate mixed solution of middle formation, after the completion of hydrazine hydrate solution injection, 40min is reacted at 40 DEG C, is searched with magnet The solid product that collection reaction generates, after which is in neutrality with the pH value of water and dehydrated alcohol alternating cleaning to cleaning solution Under nitrogen protection, dry 7h is dry in 60 DEG C.
Embodiment 4
1, a kind of preparation method of ferromagnetic nano wire, described method includes following steps:
(1) ferromagnetic metal salt (ferric nitrate) is dissolved in deionized water, is then with PH regulator (lime) tune pH value 12, stabilizer (cystine), complexing agent (sodium pyrophosphate) and surfactant (Isosorbide-5-Nitrae butynediols) are added, after stirring, is passed through Nitrogen forms nitric acid iron mixed solution to remove the oxygen in solution;Iron nitrate concentration is in the nitric acid iron mixed solution 0.1mol/L, cystine concentration 0.03mol/L, sodium pyrophosphate concentration are 0.001mol/L, and Isosorbide-5-Nitrae butynediols concentration is 0.002mol/L;
(2) after reducing agent (aluminium borohydride) being dissolved in dehydrated alcohol, aluminium borohydride solution is formed;In the aluminium borohydride solution Aluminium borohydride concentration is 1.5mol/L;
(3) syringe is used to enter step the aluminium borohydride solution formed in step (2) with the speed injection of 90mL/s (1) in the nitric acid iron mixed solution formed in, after the completion of the injection of aluminium borohydride solution, 35min is reacted at 30 DEG C, with magnet The solid product that reaction generates is collected, which is in neutrality with the pH value that water and dehydrated alcohol are alternately cleaned to cleaning solution Afterwards under nitrogen protection, dry 8h is dry in 65 DEG C.
Embodiment 5
1, a kind of preparation method of ferromagnetic nano wire, described method includes following steps:
(1) ferromagnetic metal salt (ferric sulfate) is dissolved in deionized water, pH is then adjusted with PH regulator (sodium hydroxide) Value is 10, adds stabilizer (diiodotyrosine), complexing agent (ammonium chloride) and surfactant (sulfamic acid sodium), is stirred Afterwards, nitrogen is passed through to remove the oxygen in solution, forms sulfuric acid iron mixed solution;Sulfuric acid concentration of iron in the sulfuric acid iron mixed solution For 0.09mol/L, diiodotyrosine concentration is 0.04mol/L, ammonium chloride concentration 0.001mol/L, and sulfamic acid na concn is 0.003mol/L;
(2) after reducing agent (hydrazine sulfate) being dissolved in deionized water, sulfuric acid hydrazine solution is formed;Hydrazine sulfate in the sulfuric acid hydrazine solution Concentration is 1.8mol/L;
(3) use syringe that the sulfuric acid hydrazine solution formed in step (2) is entered step (1) with the speed injection of 80mL/s In the sulfuric acid iron mixed solution of middle formation, after the completion of the injection of sulfuric acid hydrazine solution, 30min is reacted at 35 DEG C, is collected with magnet React the solid product generated, after which is in neutrality with the pH value of water and dehydrated alcohol alternately cleaning to cleaning solution Under nitrogen protection, dry 8h is dry in 60 DEG C.
Comparative example 1
The difference from embodiment 1 is that the sodium borohydride solution formed in step (2) is instilled step by the way of dropwise addition Suddenly in the ferrous sulfate heptahydrate mixed solution formed in (1).
It ferromagnetic is received under 1.75 ten thousand times and 100,000 times of amplification factor to what is prepared in embodiment 1 respectively using scanning electron microscope Rice noodles are detected, and test result is shown in Fig. 1 and Fig. 2, wherein Fig. 1 is the SEM figure under 1.75 ten thousand times, and Fig. 2 is under 100,000 times SEM figure, by Fig. 1 and Fig. 2 it is found that the ferromagnetic nano wire prepared in embodiment 1 has preferable dispersibility, and diameter exists 100nm hereinafter, length at 3~10 μm.
X-ray diffraction is carried out to the ferromagnetic nano wire prepared in embodiment 1, test result is shown in Fig. 3, from the figure 3, it may be seen that the iron The map of the diffraction maximum of magnetic nanowires and the peak value of standard diffraction map (JCPDS card no.06-0696) coincide, and illustrate to make Standby product is made of fe, and is occurred without miscellaneous peak, illustrates the purity is high of ferromagnetic nano wire in sample, is approached 100%.
Prepare the sample containing the ferromagnetic nano wire 40wt% in embodiment 1, through coaxial method within the scope of 2~18GHz into Row test, test result are shown in Fig. 4, and as shown in Figure 4, minimal reflection loss reaches -18dB, and reflection loss has less than -10dB's Effect absorption region is 7.02~9.58GHz, and range format reaches 2.56GHz, it is sufficient to be shown by the method preparation in the present invention Ferromagnetic nano wire has excellent electromagnetic shielding absorbing property.
It ferromagnetic is received under 2.79 ten thousand times and 50,000 times of amplification factor to what is prepared in embodiment 3 respectively using scanning electron microscope Rice noodles are detected, and test result is shown in Fig. 5 and Fig. 6, wherein Fig. 5 is the SEM figure under 2.79 ten thousand times, and Fig. 6 is the SEM under 50,000 times Figure, by Fig. 5 and Fig. 6 it is found that the ferromagnetic nano wire prepared in embodiment 3 has a preferable dispersibility, and diameter 100nm with Under, length is at 3~10 μm.
The ferromagnetic nano wire prepared in comparative example 1 is examined under 12.4 ten thousand times of amplification factors using scanning electron microscope It surveys, test result is shown in Fig. 7, and as shown in Figure 7, the ferromagnetic nano wire major diameter prepared in comparative example 1 is smaller and more curved It is bent.
In the present invention, in addition to using molysite, one of nickel salt or cobalt salt can also be used, identical technology is also able to achieve Effect.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be Various changes are made to it in form and in details, without departing from claims of the present invention limited range.

Claims (10)

1. a kind of preparation method of ferromagnetic nano wire, which is characterized in that described method includes following steps:
(1) ferromagnetic metal salt is soluble in water, then adjusting pH value is 10~12, adds stabilizer, complexing agent and surface Activating agent after stirring, removes the oxygen in solution, forms ferromagnetic metal mixed salt solution;The ferromagnetic metal salt mixing Ferromagnetic metal salinity is 0.05~0.15mol/L in solution, and stabilizer concentration is 0.02~0.04mol/L, and complexing agent is dense Degree is 0.001~0.002mol/L, and surfactant concentration is 0.002~0.003mol/L;
(2) after dissolving reduce agent in solution, reducing agent solution is formed;In the reducing agent solution reductant concentration be 0.9~ 2mol/L;
(3) reducing agent solution formed in step (2) is entered step to the ferromagnetic metal formed in (1) by way of injection In mixed salt solution, after the completion of reducing agent solution injection, 30~45min is reacted at 20~40 DEG C, is obtained solid and is produced Object, it is the solid product is cleaned, dry.
2. the method according to claim 1, wherein the ferromagnetic metal salt is molysite, nickel in step (1) One of salt or cobalt salt.
3. according to the method described in claim 2, it is characterized in that, the molysite is ferrous sulfate heptahydrate, frerrous chloride, sulfuric acid At least one of iron, iron chloride, ferric nitrate, ironic citrate;The nickel salt is nickel sulfate hexahydrate, nickel chloride, nickel nitrate, acetic acid At least one of nickel;The cobalt salt is at least one of cobalt chloride, cobaltous sulfate, cobalt nitrate, cobalt acetate.
4. the method according to claim 1, wherein PH regulator used is when adjusting pH value in step (1) At least one of sodium hydroxide, sodium bicarbonate, sodium carbonate, lime.
5. the method according to claim 1, wherein the stabilizer is dodecyl vinegar ammonia in step (1) At least one of acid, gelatin, cysteine, diiodotyrosine, cystine, dimethyl disulfide carbamate;The complexing agent For polyvinylpyrrolidone, glycerol, edetate, sodium ammonium triacetate, sodium pyrophosphate, ethylenediamine tetraacetic methene sodium phosphate, At least one of potassium pyrophosphate, diethylenetriamine pentacarboxylic acid salt, ammonium chloride;The surfactant is polystyrene, poly- second Glycol, sulfamic acid sodium, neopelex, 1,4 butynediols, sulfamic acid potassium, at least one in Cetrimide Kind.
6. the method according to claim 1, wherein the reducing agent is sodium borohydride, boron hydrogen in step (2) Change at least one of potassium, aluminium borohydride, hydrazine hydrate, hydrazine sulfate, formaldehyde or dimethylamino borine.
7. the method according to claim 1, wherein the solution is water, dehydrated alcohol or second in step (2) One of aqueous solution of alcohol.
8. the method according to claim 1, wherein the cleaning is specially with water and anhydrous second in step (3) The pH value that alcohol is alternately cleaned to cleaning solution is in neutrality;The drying be specially under nitrogen protection, dry 7 in 50~70 DEG C~ 9h。
9. described in any item methods according to claim 1~7, which is characterized in that in step (2), the speed of the injection is 50~90mL/s.
10. the ferromagnetic nano wire prepared by method according to any one of claims 1 to 9.
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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
CN110681873A (en) * 2019-10-16 2020-01-14 重庆邮电大学 Flexible strain sensor based on iron nanowires and preparation method thereof
CN110976898A (en) * 2019-12-12 2020-04-10 沈阳工业大学 Soft magnetic metal iron porous micron wire and preparation method thereof
CN111676548A (en) * 2020-07-21 2020-09-18 和爱电磁兼容科技(安徽)有限公司 Carbon material high-temperature wave-absorbing composite material and preparation method thereof
CN113426999A (en) * 2021-07-14 2021-09-24 重庆邮电大学 Magnetic nanowire with core-shell heterostructure and preparation method and application thereof
CN115740436A (en) * 2022-11-21 2023-03-07 重庆邮电大学 One-dimensional core-shell structure carbon-coated ferromagnetic nanowire, and preparation method and application thereof

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