CN110534329B - Preparation method of iron-nickel alloy magnetic fluid - Google Patents
Preparation method of iron-nickel alloy magnetic fluid Download PDFInfo
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- CN110534329B CN110534329B CN201910790127.0A CN201910790127A CN110534329B CN 110534329 B CN110534329 B CN 110534329B CN 201910790127 A CN201910790127 A CN 201910790127A CN 110534329 B CN110534329 B CN 110534329B
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/001—Heat treatment of ferrous alloys containing Ni
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
- H01F1/442—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a metal or alloy, e.g. Fe
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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Abstract
The invention relates to a preparation method of an iron-nickel alloy magnetic fluid, which comprises the following steps: carrying out heat treatment on the iron-nickel alloy to magnetize the iron-nickel alloy; polishing the iron-nickel alloy subjected to heat treatment to obtain iron-nickel alloy polishing solution; carrying out ultrasonic oscillation washing on the iron-nickel alloy polishing solution; carrying out centrifugal washing on the iron-nickel alloy polishing solution subjected to ultrasonic oscillation washing by using ethanol to obtain iron-nickel alloy nanosheets; activating the iron-nickel alloy nanosheets by using acetone; carrying out surface modification treatment on the activated iron-nickel alloy nanosheets and carrying out centrifugal separation; and dispersing the iron-nickel alloy nanosheets subjected to surface modification treatment in a liquid medium to obtain the iron-nickel alloy magnetic fluid. The preparation method can prepare the iron-nickel alloy magnetic fluid without adopting expensive iron-nickel alloy nano particles, reduces the preparation cost of the iron-nickel alloy magnetic fluid, and promotes the popularization and application of the iron-nickel alloy fluid.
Description
Technical Field
The invention belongs to the technical field of magnetic fluid, and particularly relates to a preparation method of iron-nickel alloy magnetic fluid.
Background
Magnetic fluid is an intelligent material with great development prospect and engineering application value, the foundation and application research in the field is widely regarded by various countries in the world in recent years, and the magnetic fluid is gradually developed into a new industry.
The magnetic fluid is also called magnetic liquid, magnetofluid and ferrofluid, and is a stable colloid system consisting of magnetic nanoparticles, carrier liquid and surfactant. Magnetic nanoparticles are nanoscale particles, and generally consist of metals such as iron, cobalt, nickel and the like, or alloys or oxides thereof.
The performance advantage of the iron-nickel alloy is that the magnetic permeability is high, and is particularly obvious under weak and medium magnetic fields. In addition, because the noble metal nickel is added, the iron-nickel alloy has extremely low coercive force and very good processing performance, and has more excellent antirust performance compared with other alloys. However, this alloy also has the disadvantage that it is expensive to produce. Because of containing elements such as nickel, cobalt, etc., the price of the alloy is generally higher.
The iron-nickel alloy magnetic nanoparticles have wide development prospect due to the characteristics of soft magnetic materials such as high saturation magnetization, high Curie temperature, high magnetic permeability, low magnetic anisotropy constant and the like, and can be applied to the fields of various materials such as high-density magnetic recording, sensors, catalysis, magnetofluid, biomedicine, pigments, electromagnetic shielding, radar wave absorption and the like.
The method for preparing the nano iron-nickel alloy is various, and the nano iron-nickel alloy is divided into three types according to the material state in the preparation process: solid phase processes, liquid phase processes and gas phase processes. The solid phase method includes mechanical alloying method, mechanochemical method, solid phase thermal decomposition method, etc. The liquid phase method includes a sol-gel method, a hydrothermal method, a liquid phase thermal decomposition method, spray pyrolysis, an electrochemical deposition method, a liquid phase reduction method, and the like. The vapor phase method includes a vapor phase chemical method, an evaporation condensation method and the like. The product obtained by physical method has low purity and uneven particle size distribution, and sometimes has high requirement on the preparation equipment, so that the preparation cost is high.
The main component for preparing the iron-nickel alloy magnetic fluid is magnetic nano iron-nickel alloy, but the application of the iron-nickel alloy fluid is limited due to the difficulty and high price of the preparation of the iron-nickel alloy nano material.
Disclosure of Invention
The invention provides a preparation method of an iron-nickel alloy magnetic fluid, which is used for solving the technical problems of high material cost and difficult popularization of the iron-nickel alloy magnetic fluid prepared from nano iron-nickel alloy in the prior art.
The first aspect of the invention provides a preparation method of an iron-nickel alloy magnetic fluid, which comprises the following steps:
carrying out heat treatment on the iron-nickel alloy to magnetize the iron-nickel alloy;
polishing the iron-nickel alloy subjected to heat treatment to obtain iron-nickel alloy polishing solution;
carrying out ultrasonic oscillation washing on the iron-nickel alloy polishing solution;
carrying out centrifugal washing on the iron-nickel alloy polishing solution subjected to ultrasonic oscillation washing by using ethanol to obtain iron-nickel alloy nanosheets;
activating the iron-nickel alloy nanosheets by using acetone;
carrying out surface modification treatment on the activated iron-nickel alloy nanosheets and carrying out centrifugal separation to obtain the iron-nickel alloy nanosheets subjected to surface modification treatment;
and dispersing the iron-nickel alloy nanosheets subjected to surface modification treatment in a liquid medium to obtain the iron-nickel alloy magnetic fluid.
Preferably, the ultrasonic vibration washing time is 5min to 10 min.
Preferably, the time for activating the nanosheets obtained by centrifugal washing is 0.5 h-2 h by using acetone.
Preferably, the time of the surface modification treatment is 20-24 h, and the reaction temperature is 25-80 ℃.
Preferably, the speed of centrifugal separation is 2000 r/min-5000 r/min, and the centrifugal time is 20 min.
Preferably, the liquid medium is one or more of DI water, ethylene glycol, fluoroether oil, or a mixture thereof.
Preferably, the thickness range of the iron-nickel alloy nanosheet is 10-50 nm, and the diameter range is 0.1-3 μm.
Preferably, the mass concentration ratio of the iron-nickel alloy nanosheet to the liquid medium is 5-30%.
As can be seen from the foregoing embodiments of the present invention, in the preparation method of an iron-nickel alloy magnetic fluid provided in the embodiments of the present application, an iron-nickel alloy is magnetized by performing heat treatment on the iron-nickel alloy, then the heat-treated iron-nickel alloy is polished to obtain a polishing solution, the polishing solution is washed and centrifuged to obtain iron-nickel alloy nanosheets, and the obtained iron-nickel alloy nanosheets are subjected to surface modification and then dispersed in a liquid medium to obtain the iron-nickel alloy magnetic fluid. Compared with the traditional preparation method, the method can prepare the iron-nickel alloy magnetic fluid without adopting expensive iron-nickel alloy nano particles, reduces the preparation cost of the iron-nickel alloy magnetic fluid, and promotes the popularization and application of the iron-nickel alloy fluid.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
Fig. 1 is a schematic flow chart of a method for preparing an iron-nickel alloy magnetic fluid according to an embodiment of the present disclosure;
fig. 2 is a scanning electron microscope image of the iron-nickel alloy magnetic fluid provided in the embodiment of the present application.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
To better understand the technical solution of the present invention, please refer to fig. 1, which is a schematic flow chart of a method for preparing an iron-nickel alloy magnetic fluid provided by the present application, the method comprising:
in the examples of the present application, since the material for preparing the iron-nickel alloy magnetic fluid is made from an iron-nickel alloy, it is required that the iron-nickel alloy has good magnetic properties. Therefore, the iron-nickel alloy material needs to be magnetized by various methods, and the heat treatment method is adopted in the embodiment of the application to magnetize the iron-nickel alloy so as to obtain the iron-nickel alloy material with excellent magnetic property.
102, polishing the iron-nickel alloy subjected to heat treatment to obtain iron-nickel alloy polishing solution;
in the embodiment of the application, the polishing of the iron-nickel alloy is not aimed at obtaining an iron-nickel alloy material with glossy surface, but is aimed at obtaining a polishing solution containing iron-nickel alloy nanosheets, so the polishing herein adopts a physical polishing method to polish the iron-nickel alloy material. And collecting the polishing solution generated by polishing.
103, carrying out ultrasonic oscillation washing on the iron-nickel alloy polishing solution;
in the embodiment of the present application, the polishing solution collected in step 102 contains more impurities, and ultrasonic oscillation washing is used to remove part of the impurities.
104, using ethanol to centrifugally wash the iron-nickel alloy polishing solution subjected to ultrasonic oscillation washing to obtain iron-nickel alloy nanosheets;
in the embodiment of the application, due to the fact that the quality of different substances in the polishing solution is different, the iron-nickel alloy nanosheets can be effectively separated from other impurities by the centrifugal method. The ethanol solution can be used for washing and cleaning organic impurities such as a polishing agent and the like adhered to the iron-nickel alloy nanosheets to obtain pure iron-nickel alloy liquid, and the pure iron-nickel alloy liquid is separated to obtain the iron-nickel alloy nanosheets. The centrifugal method can also divide the iron-nickel alloy into different thicknesses and sizes for manufacturing iron-nickel alloy magnetic fluid for different purposes.
105, activating iron-nickel alloy nanosheets by using acetone;
in the embodiment of the application, the washed iron-nickel alloy nanosheets are added to an acetone solution for activation.
106, carrying out surface modification treatment on the activated iron-nickel alloy nanosheets and carrying out centrifugal separation to obtain the iron-nickel alloy nanosheets subjected to surface modification treatment;
in the embodiment of the application, the iron-nickel alloy nanosheets activated by acetone in step 105 are added into an organic solvent for surface modification treatment, and after the treatment, the mixed solution is subjected to centrifugal separation to obtain the organic matter-coated iron-nickel alloy nanosheets.
And 107, dispersing the iron-nickel alloy nanosheets subjected to surface modification treatment into a liquid medium to obtain the iron-nickel alloy magnetic fluid.
In the embodiment of the application, the iron-nickel alloy nanosheets coated with the organic matter after the surface modification treatment are uniformly dispersed in a liquid medium, so that the iron-nickel alloy magnetic fluid can be obtained. Fig. 2 is a scanning electron microscope image of the magnetic fluid made of an iron-nickel alloy according to an embodiment of the present disclosure.
According to the preparation method of the iron-nickel alloy magnetic fluid provided by the embodiment of the application, the iron-nickel alloy is magnetized by carrying out heat treatment on the iron-nickel alloy, then the heat-treated iron-nickel alloy is polished to obtain polishing solution, the polishing solution is washed and centrifuged to obtain iron-nickel alloy nanosheets, and the obtained iron-nickel alloy nanosheets are subjected to surface modification and then are dispersed in a liquid medium to obtain the iron-nickel alloy magnetic fluid. Compared with the traditional preparation method, the method can prepare the iron-nickel alloy magnetic fluid without adopting expensive iron-nickel alloy nano particles, reduces the preparation cost of the iron-nickel alloy magnetic fluid, and promotes the popularization and application of the iron-nickel alloy fluid.
As a preferred embodiment, the time for ultrasonic vibration washing is 5min to 10 min.
In a preferred embodiment, the time for activating the nanosheets obtained by centrifugal washing is 0.5h to 2h using acetone.
In a preferred embodiment, the surface modification treatment is carried out for 20 to 24 hours at a reaction temperature of 25 to 80 ℃.
As a preferred embodiment, the speed of centrifugal separation is 2000r/min to 5000r/min, and the centrifugal time is 20 min.
As a preferred embodiment, the liquid medium is one or more mixtures of DI water, ethylene glycol, fluoroether oil.
As a preferred embodiment, the thickness of the iron-nickel alloy nanosheet is in the range of 10-50 nm, and the diameter is in the range of 0.1-3 μm.
As a preferable embodiment, the mass concentration ratio of the iron-nickel alloy nanosheet to the liquid medium is 5-30%.
Several examples are listed below for reference:
example 1:
(1) taking certain iron-nickel alloy 1J50 to carry out heat treatment, wherein the heat treatment is carried out in a hydrogen heat treatment furnace, and the basic working procedures of the heat treatment are as follows: acetone cleaning → drying → charging → cooling water → N2 furnace cleaning → H2 → electric heating → heat preservation → cooling → discharging. Keeping the temperature at 1130 ℃ for 4H, introducing H2 continuously when the temperature reaches 600 ℃, and rapidly cooling to 200 ℃.
(2) Taking the iron-nickel alloy after certain heat treatment, and polishing.
(3) And putting a certain amount of polishing solution into a 500mL beaker, pouring 200mL of absolute ethyl alcohol, performing ultrasonic oscillation washing for 10min, centrifuging, and repeatedly washing the iron-nickel alloy waste liquid for three times according to the steps to obtain the pure iron-nickel alloy liquid.
(4) And adding the washed iron-nickel alloy sheet into 100mL of acetone solution, activating for 1h, and taking out.
(5) Adding the activated iron-nickel alloy sheet liquid into 100mL of oleic acid (octadecenoic acid), stirring uniformly, and standing at 25 ℃ for 24 h.
(6) And centrifuging the iron-nickel alloy sheet liquid and the oleic acid mixed liquid at the rotating speed of 3000r/min for 20min to obtain the oleic acid coated iron-nickel alloy sheet.
(7) Uniformly dispersing the iron-nickel alloy sheet wrapped by the oleic acid in DI water to obtain the magnetic nano fluid. The magnetic fluid can be stably stored for more than 3 months, has high magnetic permeability, can rapidly and reversibly move particles in the liquid under weak and medium magnetic fields, and can rapidly and reversibly change the fluidity, viscosity and the like of the fluid.
Example 2:
the steps (1), (2), (3), (4) and (5) are the same as the example 1, and the steps (6) to (7) are as follows:
(6) and centrifuging the iron-nickel alloy sheet liquid and the oleic acid mixed liquid for 20min at the rotating speed of 4000r/min to obtain the oleic acid coated iron-nickel alloy sheet.
(7) Uniformly dispersing the iron-nickel alloy sheet wrapped by the oleic acid in a mixed solution of ethylene glycol and water to obtain the magnetic nano fluid. The magnetic fluid can be stably stored for more than 3 months, has high magnetic permeability, can rapidly and reversibly move particles in the liquid under weak and medium magnetic fields, and can rapidly and reversibly change the fluidity, viscosity and the like of the fluid.
Example 3:
the steps (1), (2), (3), (4) and (5) are the same as the example 1, and the steps (6) to (7) are as follows:
(6) and centrifuging the iron-nickel alloy sheet liquid and the oleic acid mixed liquid at the rotating speed of 5000r/min for 20min to obtain the oleic acid coated iron-nickel alloy sheet.
(7) And uniformly dispersing the iron-nickel alloy sheet wrapped by the oleic acid in the fluoroether oil to obtain the magnetic nano fluid. The magnetic fluid can stably exist for more than 1 year, has high magnetic permeability, can enable particles in liquid to rapidly and reversibly move under weak and medium magnetic fields, has high surface activity, high heat-resistant stability and high chemical stability, and has fluorine-containing hydrocarbon groups which are insoluble in water and oil, so the magnetic fluid has better effects in the aspects of sealing and lubricating applications.
In the above embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
In view of the above description of the technical solutions provided by the present invention, those skilled in the art will recognize that there may be variations in the technical solutions and the application ranges according to the concepts of the embodiments of the present invention, and in summary, the content of the present specification should not be construed as limiting the present invention.
Claims (8)
1. A method for preparing an iron-nickel alloy magnetic fluid, which is characterized by comprising the following steps:
carrying out heat treatment on the iron-nickel alloy to magnetize the iron-nickel alloy; wherein the heat treatment is carried out in a hydrogen heat treatment furnace, and the basic procedures of the heat treatment are as follows: acetone cleaning → drying → charging → cooling water → N2 furnace cleaning → H2 → electric heating → heat preservation → cooling → discharging; wherein the heat preservation step comprises the steps of preserving heat for 4 hours at the temperature of 1130 ℃, continuously introducing H2 to 600 ℃, and rapidly cooling to 200 ℃;
polishing the iron-nickel alloy subjected to heat treatment to obtain iron-nickel alloy polishing solution;
carrying out ultrasonic oscillation washing on the iron-nickel alloy polishing solution;
carrying out centrifugal washing on the iron-nickel alloy polishing solution subjected to ultrasonic oscillation washing by using ethanol to obtain iron-nickel alloy nanosheets;
activating the iron-nickel alloy nanosheets by using acetone;
carrying out surface modification treatment on the activated iron-nickel alloy nanosheets and carrying out centrifugal separation to obtain the iron-nickel alloy nanosheets subjected to surface modification treatment;
and dispersing the iron-nickel alloy nanosheets subjected to surface modification treatment in a liquid medium to obtain the iron-nickel alloy magnetic fluid.
2. The method for preparing a magnetic fluid according to claim 1, wherein the ultrasonic oscillation washing is performed for 5 to 10 min.
3. The method for preparing a magnetic fluid according to claim 1, wherein the time for activating the nanosheets obtained by centrifugal washing with acetone is 0.5 to 2 hours.
4. The method for preparing a magnetic fluid according to claim 1, wherein the surface modification treatment is performed for 20 to 24 hours at a reaction temperature of 25 to 80 ℃.
5. The method according to claim 1, wherein the centrifugation rate is 2000r/min to 5000r/min, and the centrifugation time is 20 min.
6. The method according to claim 1, wherein the liquid medium is one or more of DI water, glycol, and fluoroether oil.
7. The method for preparing a magnetic fluid according to claim 1, wherein the thickness of the iron-nickel alloy nanosheet is in a range of 10-50 nm, and the diameter is in a range of 0.1-3 μm.
8. The method for preparing a magnetic fluid according to claim 1, wherein the mass concentration ratio of the iron-nickel alloy nanosheets to the liquid medium is 5% to 30%.
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| GB458315A (en) * | 1935-07-08 | 1936-12-17 | Ig Farbenindustrie Ag | Improvements in the manufacture and production of magnetisable iron-nickel alloys |
| JPH06139547A (en) * | 1992-10-28 | 1994-05-20 | Fuji Photo Film Co Ltd | Magnetic recording medium |
| US5462685A (en) * | 1993-12-14 | 1995-10-31 | Ferrofluidics Corporation | Ferrofluid-cooled electromagnetic device and improved cooling method |
| CN1725388A (en) * | 2005-06-17 | 2006-01-25 | 同济大学 | A kind of magnetic flow liquid magnetic-particle and preparation method thereof with high antioxidant |
| CN102290186B (en) * | 2011-05-04 | 2012-12-19 | 北京科技大学 | High-concentration magnetic fluid and preparation method thereof |
| CN103333731B (en) * | 2013-06-08 | 2014-10-29 | 东南大学 | Method for preparing magnetorheological fluid |
| CN103606429B (en) * | 2013-10-17 | 2016-02-24 | 南昌大学 | A kind of nano chromium carbide ferrofluid and preparation method thereof |
| CN106486240B (en) * | 2015-08-28 | 2019-01-08 | 湖南博海新材料股份有限公司 | The Preparation equipment and method of nanometer magneto-rheological fluid |
| US10774218B2 (en) * | 2017-11-03 | 2020-09-15 | The Boeing Company | Iron particle passivation |
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