CN104368825A - Preparation method for shape-controllable ferrocobalt magnetic nanoparticles - Google Patents
Preparation method for shape-controllable ferrocobalt magnetic nanoparticles Download PDFInfo
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- CN104368825A CN104368825A CN201410678346.7A CN201410678346A CN104368825A CN 104368825 A CN104368825 A CN 104368825A CN 201410678346 A CN201410678346 A CN 201410678346A CN 104368825 A CN104368825 A CN 104368825A
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Abstract
The invention discloses a preparation method for shape-controllable ferrocobalt magnetic nanoparticles and belongs to a preparation method for magnetic nano materials. Inert gas is introduced into a mixed solution A formed by ferrous sulfate and cobalt chloride in advance, so the mixed solution A always remains under an inert gas environment; then an ultrasound operation is conducted on the mixed solution A in an ultrasonic oscillation instrument for five minutes so that ferrous sulfate and cobalt chloride can be completely dissolved, and the mixed solution A is heated until a preset temperature ranging from 60 DEG C to 100 DEG C is reached; 80wt.% of hydrazine hydrate and sodium hydroxide are added to every 100 ml of saline solutions, after a reaction occurs under the set temperature, obtained products are rinsed through the inert gas and dried, and the ferrocobalt magnetic nanoparticles are obtained. According to the method, no surface active agent is needed, platy or cubic nanoparticles can be obtained only by changing the reaction temperature, the method is simple and convenient to implement, the yield in a primary reaction is large, and the shape-controllable ferrocobalt magnetic nanoparticles have broad application prospects in the numerous fields of magnetic recording materials, microwave absorption materials, biotechnology, hard alloy materials, catalytic agent materials and the like.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic Nano material, particularly relate to a kind of preparation method of controlled shape ferrocobalt magnetic nano-particle.
Background technology
Ferrocobalt has lower magnetostriction, lower coercivity, higher resistivity, very high magnetic saturation intensity (can reach 2.45 T), higher Curie temperature and higher magnetic anisotropy etc. as a kind of soft magnetic materials.These performances make it have a wide range of applications in various fields such as magnetic recording material, microwave absorbing material, biotechnology, Hardmetal materials and catalytic materials.
In recent years, shape controlling metal nanoparticle is owing to can improve the pattern of nano particle greatly, and the impact of the pattern of nano particle on its chemistry, physics, electronics, optics, magnetic and catalytic performance causes the great interest of people.At present, researcher makes great progress in shape controlling noble metal (as silver, gold, platinum, palladium) nano particle.As document [Science, 2002,298,2176] reports the regular octahedral platinum nano particles rescinded angle hexahedron golden nanometer particle that used liquid phase method to synthesize under surfactant condition; Patent [201110105032.4] reports the regular octahedral platinum nano particles that used liquid phase method to synthesize under surfactant condition.Compared with noble metal, ferrocobalt is relatively active due to its chemical property, is therefore difficult to control the growth selection to iron cobalt nanocrystal shape.Relevant report for shape controlling ferrocobalt magnetic nano-particle is also less, and the ferrocobalt magnetic nano-particle preparing shape controlling under the condition not using surfactant remains a very large challenge, not yet has the report of this respect at present.
Summary of the invention
Technical problem to be solved by this invention there is provided a kind of technique preparation method that is simple, with low cost, energy large area synthesis controlled shape ferrocobalt magnetic nano-particle under the condition not using surfactant.
The technical solution adopted in the present invention is as follows:
A preparation method for controlled shape ferrocobalt magnetic nano-particle, it realizes as follows:
Step 1: pass into inert gas in deionized water until remove the oxygen in described deionized water, be then that ferrous sulfate and the cobalt chloride of 1:1 is dissolved in described deionized water by the ratio of molal quantity, be configured to ferrous sulfate and the cobalt chloride mixed solution A of 0.05 mol/L;
Step 2: the described mixed solution A of configuration in step 1 is placed on the ultrasonic ferrous sulfate in described mixed solution and the cobalt chloride of making in supersonic oscillations instrument and dissolves completely, then described mixed solution A is heated to predetermined temperature;
Step 3: the hydrazine hydrate and the NaOH that add 80 wt.% in the described mixed solution A of configuration in step 2 obtain mixed solution B, and adding proportion is for adding the hydrazine hydrate of 20 ml 80 wt.% and the NaOH of 5 g in mixed solution A described in every 100 ml;
Step 4: reacting phase obtains difform ferrocobalt magnetic nano-particle at once at a certain temperature:
A. after described mixed solution B obtained in step 3 being reacted 15-60 min at 60 ~ 70 DEG C, then dry gained centrifugation product is cleaned under inert gas atmosphere, just obtained described cubic ferrocobalt magnetic nano-particle;
B. after described mixed solution B obtained in step 3 being reacted 15-60 min at 70 ~ 80 DEG C, then dry gained centrifugation product is cleaned under inert gas atmosphere, just obtained described sheet and cubic ferrocobalt magnetic nano-particle;
C. after described mixed solution B obtained in step 3 being reacted 15-60 min at 80 ~ 95 DEG C, then dry gained centrifugation product is cleaned under inert gas atmosphere, just obtained described sheet shape ferrocobalt magnetic nano-particle.
Further, described step 1 passes into inert gas in deionized water and makes the oxygen content in deionized water be less than 50 ppm.
Further, the ratio adding molal quantity in described step 1 in deionized water first passes into inert gas 10 ~ 30min before being the ferrous sulfate of 1:1 and cobalt chloride in deionized water.
Further, described inert gas comprises argon gas or nitrogen or its gaseous mixture.
Further, ultrasonic under supersonic oscillations instrument in described step 2 time range is 1-10 min thus fully dissolves ferrous sulfate and cobalt chloride.
Further, the temperature range being heated to predetermined temperature in described step 2 is 60 ~ 100 DEG C.
Further, in described step 2, reaction time is at a predetermined temperature that 15 ~ 60 min are until react completely.
Further, in described step 4, the scope of design temperature is 60 ~ 100 DEG C.
Further, in the process of step 1 ~ 4, mixed solution is kept to remain under inert gas atmosphere to continuing to pass into inert gas in described deionized water.
The invention has the beneficial effects as follows:
1, the easy use of the present invention, does not need surfactant, can reduce costs, enhance productivity.
2, reducing agent used in the present invention is hydrazine hydrate, generates nitrogen and hydrogen after reaction, can not form secondary pollution and react thoroughly.
3, the present invention can change the shape of the nano particle of generation by changing reaction temperature, such as, at 60 ~ 70 DEG C, reaction can obtain cubic nano particle, at 70 ~ 80 DEG C, reaction can obtain cubic and flake nano mix particles, and at 80 ~ 100 DEG C, reaction can obtain flake nano particle.
4, primary first-order equation output of the present invention is comparatively large, has a wide range of applications in various fields such as magnetic recording material, microwave absorbing material, biotechnology, Hardmetal materials and catalytic materials.
Accompanying drawing explanation
Accompanying drawing 1 is 40,000 times of field emission scanning electron microscope photo figure of the cubic ferrocobalt nano particle that the embodiment of the present invention 1 obtains.
Accompanying drawing 2 is 150,000 times of field emission scanning electron microscope photo figure of the cubic ferrocobalt nano particle that the embodiment of the present invention 1 obtains.
Accompanying drawing 3 is the high power projection electron microscope photo figure of the cubic ferrocobalt nano particle that the embodiment of the present invention 1 obtains.
Accompanying drawing 4 be the embodiment of the present invention 1 obtain cubic ferrocobalt nano particle high power projection electron microscope photo figure in [001] tape spool choose electronic diffraction photo figure.
Accompanying drawing 5 is energy disperse spectroscopy (EDS) collection of illustrative plates of the cubic ferrocobalt nano particle that the embodiment of the present invention 1 obtains.
Accompanying drawing 6 is 150,000 times of field emission scanning electron microscope photo figure of the ferrocobalt nano particle that the sheet of the embodiment of the present invention 2 acquisition mixes with cubic.
Accompanying drawing 7 is the projection electron microscope photo figure of the shape ferrocobalt nano particle that the sheet of the embodiment of the present invention 2 acquisition mixes with cube.
Accompanying drawing 8 is 60,000 times of field emission scanning electron microscope photo figure of the sheet ferrocobalt nano particle that the embodiment of the present invention 3 obtains.
Accompanying drawing 9 is the projection electron microscope photo figure of the sheet ferrocobalt nano particle that the embodiment of the present invention 3 obtains.
Accompanying drawing 10 is energy disperse spectroscopy (EDS) collection of illustrative plates of the sheet ferrocobalt nano particle that the embodiment of the present invention 3 obtains.
Accompanying drawing 11 is that the ferrocobalt nano particle that the embodiment of the present invention 1 ~ 3 obtains divides other X ray diffracting spectrum, wherein, and the X ray diffracting spectrum of the ferrocobalt nano particle that spectral line (a) obtains for embodiment 3;
The X ray diffracting spectrum of the ferrocobalt nano particle that spectral line (b) obtains for embodiment 2;
The X ray diffracting spectrum of the ferrocobalt nano particle that spectral line (c) obtains for embodiment 1.
The ferrocobalt nano particle that accompanying drawing 12 embodiment of the present invention 1 ~ 3 obtains divides other hysteresis curve collection of illustrative plates;
Wherein, spectral line a is the hysteresis curve collection of illustrative plates of the ferrocobalt nano particle that embodiment 3 obtains;
Spectral line b is the hysteresis curve collection of illustrative plates of the ferrocobalt nano particle that embodiment 2 obtains;
Spectral line a is the hysteresis curve collection of illustrative plates of the ferrocobalt nano particle that embodiment 1 obtains.
Detailed description of the invention
For making the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly, be described in detail below in conjunction with accompanying drawing 1 ~ 12 and specific embodiment.
The implementation method of embodiment 1 is as follows:
The cobalt chloride of the ferrous sulfate of 0.05 mol/L and 0.05 mol/L is dissolved in 100 ml deionized waters and obtains mixed solution A, first inert gas is passed into before adding ferrous sulfate and cobalt chloride in deionized water, inert gas such as argon gas or nitrogen, to remove oxygen remaining in water, solution is made to remain under inert gas atmosphere, ferrous sulfate and cobalt chloride are dissolved completely described mixed solution A ultrasonic about 5 min in supersonic oscillations instrument, after described mixed solution A is heated to 60 DEG C, in described mixed solution A, add 20ml 80 wt.% again hydrazine hydrate and 5 g NaOH obtain mixed solution B.After abundant reaction 30 min, clean under inert gas atmosphere and dry gained centrifugation product, just the ferrocobalt magnetic nano-particle of obtained cubic, as shown in accompanying drawing 1 ~ 4 and accompanying drawing 9 ~ 10.
The implementation method of embodiment 2 is as follows:
The cobalt chloride of the ferrous sulfate of 0.05 mol/L and 0.05 mol/L is dissolved in 200 ml deionized waters and obtains mixed solution A, first inert gas is passed into before adding ferrous sulfate and cobalt chloride in deionized water, inert gas such as argon gas or nitrogen, to remove oxygen remaining in water, and make solution remain under inert gas atmosphere, slaine (i.e. ferrous sulfate and cobalt chloride) is dissolved completely described mixed solution A ultrasonic about 5 min in supersonic oscillations instrument, after described mixed solution is heated to 80 DEG C, in described mixed solution A, add 40ml 80 wt.% again hydrazine hydrate and 10 g NaOH obtain mixed solution B.After abundant reaction 30 min, clean and dry gained centrifugation product under protection gas, just the ferrocobalt magnetic nano-particle of obtained sheet and cubic, as shown in accompanying drawing 5 ~ 6 and accompanying drawing 9 ~ 10.
The implementation method of embodiment 3 is as follows:
The cobalt chloride of the ferrous sulfate of 0.05 mol/L and 0.05 mol/L is dissolved in 300 ml deionized waters and obtains mixed solution A, first inert gas is passed into before adding ferrous sulfate and cobalt chloride, inert gas and argon gas or nitrogen, to remove oxygen remaining in water, and make solution remain under inert gas atmosphere, ferrous sulfate and cobalt chloride are dissolved completely described mixed solution A ultrasonic about 5 min in supersonic oscillations instrument, after described mixed solution A is heated to 100 DEG C, 60 ml 80 wt.% hydrazine hydrates are added again and 15 g NaOH obtain mixed solution B to described mixed solution A.After abundant reaction 30 min, clean under inert gas atmosphere and dry gained centrifugation product, just the ferrocobalt magnetic nano-particle of obtained sheet, as shown in accompanying drawing 7 ~ 10.
From above-described embodiment, by changing reaction temperature, the shape of the ferrocobalt magnetic nano-particle just can prepared.According to classical growth theory, nanocrystalline shape determines primarily of the speed of growth of different crystal face.Classical Bravais-Friedel, Donnay-Harker (BFDH) growth model, think a certain crystal face the speed of growth (
r hkl ) and its interplanar distance (
d hkl ) inverse be directly proportional, namely
r hkl ∝ 1/
d hkl .Nanocrystalline net shape depend primarily on [100] and [111] both direction growth velocity ratio (
r).If velocity ratio (
r) less of about 0.7, so will grow exposure is { 100} face cube structure.For a cube FeCo alloy, due to
d 100 >
d 110 >
d 111 , thus the growth rate of two crystal faces is closed and is
r 100 >
r 110 >
r 111 .In addition, because { surface energy in 111} face is lower, is thus greater than the speed of growth along <100> direction along the speed of growth in <111> direction.In this chapter, velocity ratio that NaOH appropriate under 60 ° of C and hydrazine hydrate make <100> and <111> both direction grow (
r) close to 0.7, therefore generate by six { nano particles of the cubic pattern that 100} face forms 100 ° of C reactions.Along with the rising of reaction temperature, reaction speed is also accelerated thereupon, and the growth rate of the speed of growth along <111> direction is higher than along the growth rate of the speed of growth in <100> direction, the velocity ratio of therefore both direction growth (
r) increase, thus can produce laminated structure. thereupon
Use hydrazine hydrate as reducing agent in the embodiment of the present invention, generate nitrogen and hydrogen after reaction, product is purer, can not form secondary pollution and react thoroughly, energy-efficient; Volume production can be carried out; Ferrocobalt has lower magnetostriction, lower coercivity, higher resistivity, very high magnetic saturation intensity (can reach 2.45 T), higher Curie temperature (about 900 as a kind of soft magnetic materials
oand higher magnetic anisotropy etc. C).It is made to have a wide range of applications in various fields such as magnetic recording material, microwave absorbing material, biotechnology, Hardmetal materials and catalytic materials.Can find out, this method utilizes liquid phase method, by regulating the temperature of reaction system just can control the nanocrystalline orientation of growth, and not only easy use, and do not need surfactant, breach technology barriers in the past.Therefore adopt this method to control the orientation of growth of ferrocobalt nano particle, just can realize the growth selection to nanocrystalline shape.
Accompanying drawing 1 ~ 2 is that 60 ° of C react the typical field emission scanning electron microscope photo of products therefrom after 30 min, and as can be seen from the figure, product is mainly cubic pattern.Its productive rate is about 85%, by the statistical analysis more than 100 FeCo nano particles, shows that its average length is about 80 nm, consistent with XRD (Figure 11) result.Accompanying drawing 3 ~ 4 is the typical projection electron microscope photo of cubic FeCo magnetic alloy nano particle, and its length of side is 85 nm, and result is consistent with field emission scanning electron microscope photo.Choose electronic diffraction display, when electron beam is surperficial perpendicular to of cube FeCo alloy, diffraction spot is cubic structure and adjacent two faces are respectively (110) face and (200) face, can determine that tape spool is [001] direction according to diffraction spot.This result proves that six faces of cube FeCo alloy are { 100} crystal face.
While carrying out field emission microscopy observation, also the chemical composition of FeCo nano particle is analyzed, see table 1, table 1 is the atomic ratio of the different elements of the cubic ferrocobalt nano particle that the embodiment of the present invention 1 obtains, as can be seen from EDX spectrum, main containing Fe, Co and a small amount of O element in product.Wherein element than Fe/Co close to 1, consistent with adding Fe element and Co element ratio in reactant, illustrate that reduction reaction is comparatively thorough.A small amount of O element may come from that the residual of NaOH and partial oxidation cause.
The atomic ratio of different element in the cubic sample of table 1
| Peak ID (at%) | Co K | Fe K | O K |
| 30 min | 45.5 | 44.8 | 9.7 |
In order to study the impact of different temperatures on FeCo magnetic alloy nano particle pattern, when reaction temperature being brought up to respectively 80 ° of C and 100 ° C.What is interesting is, during 80 ° of C, in product, occur some cubic and sheet FeCo magnetic alloy nano particles.Accompanying drawing 6 ~ 7 is that 80 ° of C react the typical field emission scanning electron microscope of 30 min afterproduct and projection electron microscope photo, therefrom clearly can find out and be mainly sheet and cubic alloy particle.Wherein cubic particle content is about 50%.Product when its size and 60 ° of C is consistent, and length is about 80 nm, and platy particle average length is ~ 100 nm, and thickness is ~ 30 nm.During 100 ° of C, field emission scanning electron microscope analysis shows that the product of gained is hexagonal plate pattern (nanometer sheet) substantially.
Accompanying drawing 8 is typical field emission scanning electron microscope photo, therefrom clearly can find out strip-like features, and its size is comparatively even.By the statistical analysis to nearly 100 FeCo nanometer sheet, show that its average length is for ~ 100 nm, thickness is ~ 30 nm.It is hexagonal plate pattern (with reference to accompanying drawing 9) that projection electron microscope demonstrates FeCo magnetic alloy further, consistent with field emission scanning electron microscope photographic result.This demonstrates the hexagonal plate structure of FeCo magnetic alloy nano particle further.
In order to further investigate the micro-structural of FeCo magnetic alloy nano particle under different temperatures, having carried out EDX constituent analysis and having characterized, see table 2 to product, table 2 be the atomic ratio of the different elements of the cubic ferrocobalt nano particle of the embodiment of the present invention 3 acquisition.
The atomic ratio of different element in table 2 platy particle
| Peak ID (at%) | Co K | Fe K | O K |
| 30 min | 46.8 | 45.7 | 7.5 |
FeCo magnetic alloy nano particle EDS analysis result, prepared platy particle contains Fe, Co O and C element.And the atomic ratio of Fe and Co is about 1:1, wherein C and O element mainly comes from that graphite conductive adhesive and partial oxidation cause.Show that obtained nanometer sheet is purer FeCo nano particle.The EDS result of 80 ° of C products therefroms and 100 ° of C be the constituent class of product seemingly.
Accompanying drawing 11 is the X ray diffracting spectrum of FeCo magnetic alloy particle prepared under different temperatures.As can be seen from collection of illustrative plates, FeCo magnetic alloy is polycrystalline structure, and 2
θ=44.8 °, 2
θ=65.3 ° and 2
θthe diffraction maximum at=64.0 ° of places corresponds respectively to characteristic diffraction peak (110), (200) and (211) of cube FeCo, reference standard diffraction card cube FeCo (JCPDS card number: 49-1568), can determine that this magnetic alloy has FeCo cubic structure.
From accompanying drawing 11 collection of illustrative plates, find out that it does not have impurity peaks in addition, show that products therefrom is purer.Do not occur the characteristic peak of metallic iron or cobalt in diffraction maximum, if product is not exist with alloy form, then have the appearance of iron or cobalt diffraction maximum, this result confirms that product is that homogeneous alloy form exists.In addition, the characteristic diffraction peak that sample is stronger, shows that the sample obtained has higher degree of crystallinity.According to (110) diffraction maximum, shown by Scherrer formulae discovery crystallite dimension, under result shows 60 ° of C conditions, FeCo magnetic alloy crystallite dimension is about 80 nm.
The hysteresis curve collection of illustrative plates of FeCo nano particle of accompanying drawing 12 for obtaining under condition of different temperatures.Wherein, when reaction temperature is 60 ° of C cubic FeCo nano particle saturation magnetization (
m s), remanent magnetism (
m r) and coercivity (H
c) Oe is respectively 139 emu/g, 14 emu/g and 180 Oe.The magnetic parameter of three kinds of different-shapes is as shown in table 3, and table 3 is the magnetic parameter of different-shape FeCo nano particle.
Wherein sheet FeCo nano particle
m scomparatively high under other two conditions, this is because product degree of crystallinity synthesized during 100 ° of C is high.The rare difference of coercivity of three kinds of samples may be because its different pattern and shape anisotropic cause.It may be noted that time, the saturation magnetization of block FeCo alloy (
m s) be 225 emu/g.In this chapter, three kinds of products are all compared with block
m slow, this is because product is caused by nanoscale.
The above embodiment is only the preferred embodiments of the present invention, and and the feasible enforcement of non-invention exhaustive.For persons skilled in the art, to any apparent change done by it under the prerequisite not deviating from the principle of the invention and spirit, all should be contemplated as falling with within claims of the present invention.
Claims (10)
1. a preparation method for controlled shape ferrocobalt magnetic nano-particle, is characterized in that: it comprises the steps:
Step 1: pass into inert gas in deionized water until remove the oxygen in described deionized water, be then that ferrous sulfate and the cobalt chloride of 1:1 is dissolved in described deionized water by the ratio of molal quantity, be configured to the mixed solution A of 0.05 mol/L ferrous sulfate and 0.05 mol/L cobalt chloride;
Step 2: the described mixed solution A of configuration in step 1 is placed on the ultrasonic ferrous sulfate in described mixed solution A and the cobalt chloride of making in supersonic oscillations instrument and dissolves completely, then described mixed solution A is heated to predetermined temperature;
Step 3: the hydrazine hydrate and the NaOH that add 80 wt.% in the described mixed solution A of configuration in step 2 obtain mixed solution B, and adding proportion is for adding the hydrazine hydrate of 20 ml 80 wt.% and the NaOH of 5 g in mixed solution A described in every 100 ml;
Step 4: after the described mixed solution B being added with hydrazine hydrate and NaOH in step 3 is reacted 15-60 min at a set temperature, centrifugal (2000rmp) 10min under inert gas atmosphere, then cleaning-drying gained centrifugation product, just obtained described controlled shape ferrocobalt magnetic nano-particle.
2. the preparation method of a kind of controlled shape ferrocobalt magnetic nano-particle according to claim 1, is characterized in that: described step 1 passes into inert gas in deionized water makes the oxygen content in deionized water be less than 50 ppm.
3. the preparation method of a kind of controlled shape ferrocobalt magnetic nano-particle according to claim 1, it is characterized in that: the ratio adding molal quantity in described step 1 in deionized water first passes into inert gas 10 ~ 30min before being the ferrous sulfate of 1:1 and cobalt chloride in deionized water.
4. the preparation method of a kind of controlled shape ferrocobalt magnetic nano-particle according to claim 1, is characterized in that: described inert gas comprises argon gas or nitrogen or its gaseous mixture.
5. the preparation method of a kind of controlled shape ferrocobalt magnetic nano-particle according to claim 1, is characterized in that: time range ultrasonic under supersonic oscillations instrument in described step 2 is 1-10 min thus fully dissolves ferrous sulfate and cobalt chloride.
6. the preparation method of a kind of controlled shape ferrocobalt magnetic nano-particle according to claim 1, is characterized in that: the temperature range being heated to predetermined temperature in described step 2 is 60 ~ 100 DEG C.
7. the preparation method of a kind of controlled shape ferrocobalt magnetic nano-particle according to claim 1, is characterized in that: in described step 2, reaction time is at a predetermined temperature that 15 ~ 60 min are until react completely.
8. the preparation method of a kind of controlled shape ferrocobalt magnetic nano-particle according to claim 1, is characterized in that: in described step 4, the scope of design temperature is 60 ~ 100 DEG C.
9. the preparation method of a kind of controlled shape ferrocobalt magnetic nano-particle according to claim 8, is characterized in that: in described step 4, design temperature is different, and between reacting phase is seasonable, obtained ferrocobalt magnetic nano-particle shape is different:
A. after described mixed solution obtained in step 3 being reacted 15-60 min at 60 ~ 70 DEG C, then dry products therefrom is cleaned under inert gas atmosphere, just obtained described cubic ferrocobalt magnetic nano-particle;
B. after described mixed liquor obtained in step 3 being reacted 15-60 min at 70 ~ 80 DEG C, then dry products therefrom is cleaned under inert gas atmosphere, just obtained described sheet and cubic ferrocobalt magnetic nano-particle;
C. after described mixed liquor obtained in step 3 being reacted 15-60 min at 80 ~ 95 DEG C, then dry products therefrom is cleaned under inert gas atmosphere, just obtained described sheet shape ferrocobalt magnetic nano-particle.
10. the preparation method of a kind of controlled shape ferrocobalt magnetic nano-particle according to claim 1, is characterized in that: in the process of step 1 ~ 4, keep mixed solution to remain under inert gas atmosphere to continuing to pass into inert gas in described deionized water.
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| CN108723383A (en) * | 2017-04-13 | 2018-11-02 | 中国科学院金属研究所 | A kind of controllable method for preparing of multiform looks, ferrocobalt magnetic nanoparticle with high saturated magnetic induction |
| CN108788126A (en) * | 2018-06-20 | 2018-11-13 | 陕西理工大学 | A kind of preparation method of cobalt nano magnetic material |
| CN113441729A (en) * | 2021-06-25 | 2021-09-28 | 东北大学 | Method for directly synthesizing high-coercivity non-noble metal nanowire by wet chemical method |
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| CN108788126A (en) * | 2018-06-20 | 2018-11-13 | 陕西理工大学 | A kind of preparation method of cobalt nano magnetic material |
| CN113441729A (en) * | 2021-06-25 | 2021-09-28 | 东北大学 | Method for directly synthesizing high-coercivity non-noble metal nanowire by wet chemical method |
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