CN107424716A - Magnetic liquid and preparation method thereof - Google Patents
Magnetic liquid and preparation method thereof Download PDFInfo
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- CN107424716A CN107424716A CN201710743951.1A CN201710743951A CN107424716A CN 107424716 A CN107424716 A CN 107424716A CN 201710743951 A CN201710743951 A CN 201710743951A CN 107424716 A CN107424716 A CN 107424716A
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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
- H01F1/445—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 compound, e.g. Fe3O4
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Abstract
The invention provides magnetic liquid and preparation method thereof.The magnetic liquid includes：Magnetic nanoparticle and K Na alloy-based carrier fluids, wherein, the magnetic nanoparticle has inner core and shell, and the shell is coated at least a portion outer surface of the inner core, and the material for forming the inner core is Fe3O4Magnetic nanoparticle, the material for forming the shell are selected from Au, Ag, Pt and SiO2At least one of.Thus the K Na alloy magnetic liquids, use temperature range is wide, and the coefficient of heat conduction is high, and saturation magnetization is high, corrosion-resistant, and plays a part of sealing, cooling and lubrication simultaneously.
Description
Technical field
The present invention relates to Material Field, specifically, being related to magnetic liquid and preparation method thereof.
Background technology
Magnetic liquid is a kind of Nano-function thin films, while has magnetic and mobility.Different, the magnetic according to base load liquid
Property liquid can be divided into：The type magnetic such as water base, keryl, gasoline base, synthetic ester base, polyglycols base, polyphenyl ether, hydrocarbons base
Property liquid.Surfactant and base load liquid are hydrocarbon type organic in existing magnetic liquid, and this kind of magnetic liquid can not be
Used within the scope of wider temperature, heat transfer coefficient is small, and radiating efficiency is low, and can not play sealing, cooling and lubrication simultaneously and make
With so as to limit its application.
Thus, current magnetic liquid still has much room for improvement.
The content of the invention
It is contemplated that at least solves one of technical problem in correlation technique to a certain extent.Therefore, the present invention
One purpose is to propose that a kind of use temperature range is wide, heat conduction efficiency is high, saturation magnetization is high or can play simultaneously
The magnetic liquid of sealing, cooling and lubrication.
The present invention is following discovery based on inventor and understanding and completed：
Inventor has found that the surfactant and base load fluidity matter being made up of hydrocarbon type organic are unstable in research process
It is fixed, by thermal decomposition magnetic liquid will be caused to fail typically more than 300 DEG C, magnetic liquid use temperature range is narrowed.Together
When, the magnetic liquid heat transfer coefficient prepared using such surfactant and base load liquid is small, and radiating efficiency is low, is using the magnetic
, it is necessary to which other auxiliary equipments maintain the normal work of magnetic liquid in liquid process, and then its application is limited, and above-mentioned magnetic
Property liquid can not play a part of simultaneously sealing, cooling and lubrication.Therefore, in view of the above-mentioned problems, inventor is deeply ground
Study carefully, propose by by magnetic nanoparticle and the compound magnetic liquid for preparing function admirable of K-Na alloy-based carrier fluids, Jin Ertuo
Its wide application.
In view of this, in one aspect of the invention, the invention provides a kind of magnetic liquid.According to the implementation of the present invention
Example, the magnetic liquid include：Magnetic nanoparticle and K-Na alloy-based carrier fluids, wherein, the magnetic nanoparticle has inner core
And shell, the shell are coated at least a portion outer surface of the inner core, the material for forming the inner core is Fe3O4Magnetic
Property nano particle (or ferroferric oxide magnetic nanoparticle), formed the shell material be selected from Au, Ag, Pt and SiO2
At least one of.Inventor has found, passes through compound, the magnetic of acquisition by the magnetic nanoparticle and K-Na alloy-based carrier fluids
Liquid can have good magnetic and mobility concurrently, and use temperature range is wide, can be competent at use demand under particular surroundings, and heat passes
Coefficient height is led, good conductivity is corrosion-resistant, can play a part of sealing, cooling and lubrication simultaneously, so as to for atomic energy core
Reactor or other military industry fields, and solve the industry visual plant long-term existence such as Aero-Space, machinery, chemical industry, pharmacy, biology
Sealing, cooling and lubrication the problems such as.
In addition, magnetic liquid according to the above embodiment of the present invention can also have technical characteristic additional as follows：
According to an embodiment of the invention, the magnetic nanoparticle is selected from Fe3O4/ Au magnetic nanoparticles, Fe3O4/Ag
Magnetic nanoparticle, Fe3O4/ Pt magnetic nanoparticles and Fe3O4/SiO2At least one of magnetic nanoparticle.Thus, obtain
Magnetic nanoparticle can be magnetized rapidly under externally-applied magnetic field and magnetic disappears immediately after removing externally-applied magnetic field, and containing upper
The magnetic liquid saturation magnetization height of magnetic nanoparticle is stated, the coefficient of heat conduction is high, and good conductivity is corrosion-resistant.
According to an embodiment of the invention, the Fe3O4/ Au magnetic nanoparticles, Fe3O4/ Ag magnetic nanoparticles, Fe3O4/
Pt magnetic nanoparticles and Fe3O4/SiO2The mass ratio of magnetic nanoparticle and the K-Na alloy-baseds carrier fluid is respectively 0.56~
5.59:1,0.4~4.03:1,0.59~5.94:1 and 0.26~2.62:1.Thus, in the range of aforementioned proportion, according to this hair
The saturation magnetization of the magnetic liquid of bright embodiment is high, and the coefficient of heat conduction is high, and good conductivity is corrosion-resistant.
According to an embodiment of the invention, the K-Na alloy-baseds carrier fluid is the alloy of sodium (Na) and potassium (K), is protected in argon gas
The sodium newly cut open and potassium are mixed to get under shield, wherein, the specific ratio of sodium and potassium is not particularly limited, art technology
Personnel can flexibly select as needed, in some embodiments of the invention, according to mass fraction meter, K-Na alloy-based carrier fluids
Sodium containing 78% potassium and 22%.Thus, K-Na alloy-baseds carrier fluid fusing point is low, and boiling point is high, and density is low, have low-steam pressure and
High thermal conductivity coefficient, be advantageous to improve the performance of magnetic liquid.
According to an embodiment of the invention, the temperature in use of the magnetic liquid is -11~785 DEG C.Thus, it is possible to competent pole
Hold the use demand under particular surroundings, can at -11~785 DEG C long-term stable operation, without volatilizing, freeze or
The problem of base load liquid and surfactant crack and lose use value.
According to an embodiment of the invention, the saturation magnetization of the magnetic liquid is 1~470Gs.Thus, it is possible to meet
The requirement of a variety of different magnetic field conditions, it is applied widely.
In another aspect of this invention, the present invention proposes a kind of method for preparing foregoing magnetic liquid.According to
Embodiments of the invention, this method include：Magnetic nanoparticle is formed, the magnetic nanoparticle has inner core and shell, institute
State shell to be coated at least a portion outer surface of the inner core, the material for forming the inner core is Fe3O4Magnetic Nano
Grain, the material for forming the shell are selected from Au, Ag, Pt and SiO2At least one of；By the magnetic nanoparticle and K-
Na alloy-baseds carrier fluid mixes.Thus, preparation method is simply easily achieved, and yield is high, low for equipment requirements.
In addition, the preparation method of magnetic liquid according to the above embodiment of the present invention can also have technology additional as follows
Feature：
According to an embodiment of the invention, the formation magnetic nanoparticle is included in following (1), (2), (3) and (4) extremely
It is one of few：(1) make the solution containing ferrous ion and iron ion and the mixed reaction of ammoniacal liquor, obtain ferroferric oxide magnetic nano
Grain, make the ferroferric oxide magnetic nanoparticle successively with HAuCl4And NH2OHHCl reacts, and obtains Fe3O4/ Au magnetic is received
Rice grain；(2) make the solution containing ferrous ion and iron ion and the mixed reaction of ammoniacal liquor, obtain ferroferric oxide magnetic nano
Grain, make the ferroferric oxide magnetic nanoparticle successively with AgNO3And NH2OHHCl reacts, and obtains Fe3O4/ Ag magnetic is received
Rice grain；(3) mixture of diacetyl acetone platinum and phenyl ether, polyethylene glycol, oleic acid and oleic acid amine is reacted, and by obtained by
Product and praseodynium iron react, obtain Fe3O4/ Pt magnetic nanoparticles；(4) make containing ferrous ion and iron ion
Solution and the mixed reaction of ammoniacal liquor, obtain ferroferric oxide magnetic nanoparticle, make the ferroferric oxide magnetic nanoparticle and four
The mixture of ammonium hydroxide and tetraethyl orthosilicate reacts, and obtains Fe3O4/SiO2Magnetic nanoparticle.Thus, preparation method
Simply it is easily achieved, yield is high.
According to an embodiment of the invention, described (1) further comprises：It is Fe according to molar ratio2+:Fe3+=1:1.5~2
The configuration solution containing ferrous ion and iron ion, control bath temperature stir at 30~90 DEG C, in molar ratio example Fe3 +:Ammoniacal liquor=1:4~8 slowly pour into 25 mass % concentrated ammonia liquor, continue to stir 5~30min of precipitation reaction in water-bath, obtain
Fe3O4Magnetic nanoparticle, by the Fe3O4Magnetic nanoparticle is dissolved in 0.1mol/L TMAH, is used
0.1mol/L sodium citrate cleaning 10min, according to the Fe3O4Magnetic nanoparticle:HAuCl4Mass ratio is 1:8~0.3 add
Enter 1 mass % HAuCl4Solution, then according to mass ratio HAuCl4:NH2OHHCl=1:2.5~6 add NH2OHHCl,
Reduction reaction 2 hours, produces the Fe3O4/ Au magnetic nanoparticles.Thus, preparation method is simply easily achieved, and yield is high.
According to an embodiment of the invention, described (2) further comprise：It is Fe according to molar ratio2+:Fe3+=1:1.5~2
The configuration solution containing ferrous ion and iron ion, control bath temperature stir at 30~90 DEG C, in molar ratio example iron
Ion:Ammoniacal liquor=1:4~8 slowly pour into 25 mass % concentrated ammonia liquor, continue to stir 5~30min of precipitation reaction in water-bath, obtain
To Fe3O4Magnetic nanoparticle, by the Fe3O4Magnetic nanoparticle is dissolved in 0.1mol/L TMAH, is adopted
10min is cleaned with 0.1mol/L sodium citrate, according to the Fe3O4Magnetic nanoparticle:AgNO3Mass ratio is 1:3.2~
0.1 adds 1 mass % AgNO3Solution, then according to mass ratio AgNO3:NH2OHHCl=1:0.8~2 adds NH2OH·
HCl, reduction reaction 2 hours, produces the Fe3O4/ Ag magnetic nanoparticles.Thus, preparation method is simply easily achieved, yield
It is high.
According to an embodiment of the invention, described (3) further comprise：In 200ml phenyl ethers, successively addition 10~
20mol polyethylene glycol -200,1~8mol of oleic acid, oleic acid 1~10mol of amine, then 1~5mol of diacetyl acetone platinum is dissolved in
In the obtained mixture containing phenyl ether, and 40~80min is reacted under the conditions of 150 DEG C, continues to be warming up to 180~200 DEG C,
According to praseodynium iron：Diacetyl acetone platinum=1:1.2~1.4 molar ratio adds praseodynium iron, keeps constant temperature
Continue 50~70min of reaction and obtain the Fe3O4/ Pt magnetic nanoparticles.Thus, preparation method is simply easily achieved, yield
It is high.
According to an embodiment of the invention, described (4) further comprise：It is Fe according to molar ratio2+：Fe3+=1：1.5~2
The configuration solution containing ferrous ion and iron ion, control bath temperature stir at 30~90 DEG C, in molar ratio example Fe3 +:Ammoniacal liquor=1:4~8 slowly pour into 25 mass % concentrated ammonia liquor, continue to stir 5~30min of precipitation reaction in water-bath, obtain
Fe3O4Magnetic nanoparticle, by the Fe3O4Magnetic nanoparticle is dissolved in 200ml TMAHs and ultrasonic disperse
10~30min, according to mass ratio Fe3O4:Tetraethyl orthosilicate=2.4~7.2:1 adds tetraethyl orthosilicate, stirring reaction 4 at 25 DEG C
~8 hours, obtain the Fe3O4/SiO2Magnetic nanoparticle.Thus, preparation method is simply easily achieved, and yield is high.
According to an embodiment of the invention, described mix the magnetic nanoparticle and K-Na alloy-baseds carrier fluid includes：In
Under anhydrous and oxygen-free, argon gas protection environment, the magnetic nanoparticle and the K-Na alloy-baseds carrier fluid are immersed in paraffin oil, water
Bath is heated slowly to 30~70 DEG C, and gentle, intermittence is stirred until homogeneous mixing, removes upper liquid, obtains the magnetic liquid.By
This, reaction condition is gentle, simple to operate, be easily achieved and control, and the magnetic liquid use temperature range obtained is wide, energy
Use demand under enough competent particular surroundings, the coefficient of heat conduction is high, and good conductivity is corrosion-resistant, sealing can be played simultaneously, cool down and
The effect of lubrication, so as to for atomic energy nuclear reactor or other military industry fields, and solve Aero-Space, machinery, chemical industry, system
The problems such as long-standing sealing of the industry visual plant such as medicine, biology, cooling and lubrication.
Brief description of the drawings
Fig. 1 is Fe in the embodiment of the present invention 2 (4)3O4TEM (transmission electron microscope) figure of magnetic nanoparticle.
Fig. 2 is only to contain Fe in the embodiment of the present invention 23O4/SiO2The K-Na alloy based magnetic liquids of magnetic nanoparticle
Magnetization curve.
Fig. 3 is that one embodiment of the invention prepares magnetic liquid schematic flow sheet.
Embodiment
Embodiments of the invention are described below in detail.The embodiments described below is exemplary, is only used for explaining this hair
It is bright, and be not considered as limiting the invention.Unreceipted particular technique or condition in embodiment, according to text in the art
Offer described technology or condition or carried out according to product description.Agents useful for same or the unreceipted production firm person of instrument,
For the conventional products of acquisition purchased in market can be passed through.
In one aspect of the invention, the invention provides a kind of magnetic liquid.According to an embodiment of the invention, the magnetic
Liquid includes：Magnetic nanoparticle and K-Na alloy-based carrier fluids, the magnetic nanoparticle have inner core and shell, the shell
It is coated at least a portion outer surface of the inner core, the material for forming the inner core is Fe3O4Magnetic nanoparticle, formed
The material of the shell is selected from Au, Ag, Pt and SiO2At least one of.Inventor has found, by by magnetic nanoparticle
It is compound with K-Na alloy-based carrier fluids, the magnetic of solid material and the mobility of fluent material can be had concurrently, magnetic liquid uses temperature
It is wide to spend scope, use demand under particular surroundings can be competent at, the coefficient of heat conduction is high, and good conductivity is corrosion-resistant, can play simultaneously
Sealing, cooling and the effect of lubrication, so as to for atomic energy nuclear reactor or other military industry fields, and solve Aero-Space,
The problems such as long-standing sealing of the industry visual plant such as machinery, chemical industry, pharmacy, biology, cooling and lubrication.
According to an embodiment of the invention, in order that obtaining magnetic liquid has preferable performance, it is desirable to the magnetic of use
Magnetic disappears immediately after nano particle is magnetized rapidly under externally-applied magnetic field and removes externally-applied magnetic field.In some implementations of the present invention
In example, the magnetic nanoparticle is selected from Fe3O4/ Au magnetic nanoparticles, Fe3O4/ Ag magnetic nanoparticles, Fe3O4/ Pt magnetic
Property nano particle and Fe3O4/SiO2At least one of magnetic nanoparticle.Thus, the magnetic nanoparticle obtained can be outside
Magnetic after being magnetized rapidly under magnetic field and removing externally-applied magnetic field is added to disappear immediately, and magnetic liquid according to embodiments of the present invention is satisfied
High with the intensity of magnetization, the coefficient of heat conduction is high, and good conductivity is corrosion-resistant.
It should be noted that describing mode " Fe used herein3O4/ Au magnetic nanoparticles " refer to nucleocapsid
The magnetic nanoparticle of structure, wherein, Fe3O4Inner core is formed, Au forms at least a portion outer surface that shell is coated on inner core
On, similar description " Fe herein3O4/ Ag magnetic nanoparticles ", " Fe3O4/ Pt magnetic nanoparticles " and " Fe3O4/SiO2Magnetic
Property nano particle " represent implication and " Fe3O4/ Au magnetic nanoparticles " are identical.
According to an embodiment of the invention, the raw material proportioning of inner core and shell is not particularly limited in magnetic nanoparticle, only
Shell can be made to be coated at least a portion outer surface of inner core, those skilled in the art can flexibly select as needed
Select.In some embodiments of the invention, Fe3O4The mass ratio of material of the magnetic nanoparticle with forming Au shells can be 1:8
~0.3；Fe3O4The mass ratio of material of the magnetic nanoparticle with forming Ag shells can be 1:3.2~0.1；Form Fe3O4Magnetic
Property nano particle material with formed Pt shells material mol ratio can be 1:1.2~1.4；Fe3O4Magnetic nanoparticle with
Form SiO2The mass ratio of the material of shell can be 2.4~7.2:1.Thus, the magnetic nanoparticle usability prepared
Preferably, and it can meet the requirement under different condition, use range is more extensive, if matching too high or too low effect
It is undesirable.
According to an embodiment of the invention, the proportioning of magnetic nanoparticle and K-Na alloy-based carrier fluids is not particularly limited, only
Meet requirement, those skilled in the art can flexibly select.In some embodiments of the invention, the Fe3O4/Au
Magnetic nanoparticle, Fe3O4/ Ag magnetic nanoparticles, Fe3O4/ Pt magnetic nanoparticles and Fe3O4/SiO2Magnetic nanoparticle
Mass ratio with the K-Na alloy-baseds carrier fluid is respectively 0.56~5.59:1,0.4~4.03:1,0.59~5.94:1 and 0.26
~2.62:1.Thus, in the range of said ratio, the magnetic liquid coefficient of heat conduction is high, and good conductivity is corrosion-resistant, can be simultaneously
Play a part of sealing, cooling and lubrication；If the too high levels of magnetic nanoparticle, the magnetic liquid prepared is unstable
It is fixed, it may occur however that magnetic nanoparticle is separated out and solid-liquid layering, magnetic liquid performance are damaged；If the content of magnetic nanoparticle
Too low, then the magnetic liquid saturation magnetization prepared is too low, and magnetic liquid can not produce response enough to externally-applied magnetic field, lose
Controllability of the demagnetizing field to magnetic liquid.
According to an embodiment of the invention, the temperature in use of the magnetic liquid is -11~785 DEG C.Thus, magnetic liquid
Property is stable, the use demand that can be competent under extreme particular surroundings, and the long-term stable operation at -11~785 DEG C, without
The problem of there is volatilization, icing or base load liquid and surfactant cracking and losing use value.
According to an embodiment of the invention, by adjusting Fe3O4/ Au magnetic nanoparticles, Fe3O4/ Ag magnetic nanoparticles,
Fe3O4/ Pt magnetic nanoparticles or Fe3O4/SiO2The proportioning of magnetic nanoparticle and K-Na alloy-based carrier fluids, can be very wide
In the range of adjust the saturation magnetization of magnetic liquid according to embodiments of the present invention, to meet to make under different use conditions
With requiring.In some embodiments of the invention, the saturation magnetization of the magnetic liquid is 1~470Gs.Thus, it is possible to
The saturation magnetization of magnetic liquid is adjusted flexibly according to use condition, and then can meet that the use of different operating environment will
Ask, use range is extensive.
In another aspect of this invention, the present invention proposes a kind of method for preparing foregoing magnetic liquid.According to
Embodiments of the invention, reference picture 3, this method includes：
S100：Magnetic nanoparticle is formed, the magnetic nanoparticle has inner core and shell, and the shell is coated on institute
State at least a portion outer surface of inner core.
According to an embodiment of the invention, in order that obtaining magnetic nanoparticle has preferable performance, formed in described
The material of core can be Fe3O4Magnetic nanoparticle, the material for forming the shell can be selected from Au, Ag, Pt and SiO2In
It is at least one.Thereby, it is possible to form nucleocapsid protection structure, preparation method is simply easily achieved, and yield is high, and can be in additional magnetic
Magnetic disappears immediately after being magnetized rapidly off field and removing externally-applied magnetic field, meets the use of some special circumstances and equipment well
It is required that.
According to an embodiment of the invention, the magnetic nanoparticle used in above-mentioned magnetic liquid can be a kind of magnetic Nano
Particle, or the mixture of a variety of magnetic nanoparticles, accordingly, the method for forming magnetic nanoparticle can be one
Kind, or it is a variety of.In some embodiments of the invention, the magnetic nanoparticle that can be used is selected from Fe3O4/ Au magnetic
Property nano particle, Fe3O4/ Ag magnetic nanoparticles, Fe3O4/ Pt magnetic nanoparticles and Fe3O4/SiO2In magnetic nanoparticle
At least one.Accordingly, forming the method for magnetic nanoparticle includes forming Fe3O4/ Au magnetic nanoparticles, Fe3O4/Ag
Magnetic nanoparticle, Fe3O4/ Pt magnetic nanoparticles and Fe3O4/SiO2At least one of method of magnetic nanoparticle.Under
It is described in detail to form Fe respectively in face3O4/ Au magnetic nanoparticles, Fe3O4/ Ag magnetic nanoparticles, Fe3O4/ Pt magnetic Nanos
Grain and Fe3O4/SiO2The specific method of magnetic nanoparticle.
According to an embodiment of the invention, Fe is formed3O4/ Au magnetic nanoparticles can be carried out by following steps：Make containing
The solution of ferrous ion and iron ion and the mixed reaction of ammoniacal liquor, obtain ferroferric oxide magnetic nanoparticle, make four oxidation three
Ferromagnetic nanoparticle successively with HAuCl4And NH2OHHCl reacts, and obtains Fe3O4/ Au magnetic nanoparticles, thereby, it is possible to
Nucleocapsid protection structure is formed, preparation method is simply easily achieved, and yield is high.
According to some specific embodiments of the present invention, Fe is formed3O4/ Au magnetic nanoparticles can be entered by following steps
OK：It is Fe according to molar ratio2+:Fe3+=1:1.5~2 configurations solution containing ferrous ion and iron ion, controls water
Bath temperature stirs at 30~90 DEG C, in molar ratio example Fe3+:Ammoniacal liquor=1:4~8 slowly pour into 25 mass % concentrated ammonia liquor,
Continue to stir 5~30min of precipitation reaction in water-bath, obtain Fe3O4Magnetic nanoparticle, by the Fe3O4Magnetic nanoparticle is molten
Solution cleans 10min in 0.1mol/L TMAH, using 0.1mol/L sodium citrate, according to the Fe3O4Magnetic
Property nano particle:HAuCl4Mass ratio is 1:8~0.3 add 1 mass % HAuCl4Solution, then according to mass ratio HAuCl4:
NH2OHHCl=1:2.5~6 add NH2OHHCl, reduction reaction 2 hours, produces the Fe3O4/ Au magnetic nanoparticles.
Thus, preparation method is simply easily achieved, and yield is high.
According to an embodiment of the invention, Fe is formed3O4/ Ag magnetic nanoparticles can be carried out by following steps：Make containing
The solution of ferrous ion and iron ion reacts with ammoniacal liquor, obtains ferroferric oxide magnetic nanoparticle, makes the ferroso-ferric oxide
Magnetic nanoparticle successively with AgNO3And NH2OHHCl reacts, and obtains Fe3O4/ Ag magnetic nanoparticles, thereby, it is possible to formed
Nucleocapsid protection structure, preparation method are simply easily achieved, and yield is high.
According to some specific embodiments of the present invention, Fe is formed3O4/ Ag magnetic nanoparticles can be entered by following steps
OK：It is Fe according to molar ratio2+:Fe3+=1:1.5~2 configurations solution containing ferrous ion and iron ion, controls water
Bath temperature stirs at 30~90 DEG C, in molar ratio example iron ion:Ammoniacal liquor=1:4~8 slowly pour into 25 mass % dense ammonia
Water, continue to stir 5~30min of precipitation reaction in water-bath, obtain Fe3O4Magnetic nanoparticle, by the Fe3O4Magnetic Nano
Grain is dissolved in 0.1mol/L TMAH, 10min is cleaned using 0.1mol/L sodium citrate, according to described
Fe3O4Magnetic nanoparticle:AgNO3Mass ratio is 1:3.2~0.1 add 1 mass % AgNO3Solution, then according to mass ratio
AgNO3:NH2OHHCl=1:0.8~2 adds NH2OHHCl, reduction reaction 2 hours, produces the Fe3O4/ Ag magnetic Nanos
Particle.Thus, preparation method is simply easily achieved, and yield is high.
According to an embodiment of the invention, Fe is formed3O4/ Pt magnetic nanoparticles can be carried out by following steps：By diethyl
Acyl acetone platinum and phenyl ether, polyethylene glycol, the mixture of oleic acid and oleic acid amine react, and by resulting product and triacetyl third
Ketone iron reacts, and obtains Fe3O4/ Pt magnetic nanoparticles, thereby, it is possible to form nucleocapsid protection structure, preparation method is simply easy to real
Existing, yield is high.
According to some specific embodiments of the present invention, Fe is formed3O4/ Pt magnetic nanoparticles can be entered by following steps
OK：In 200ml phenyl ethers, 10~20mol polyethylene glycol -200,1~8mol of oleic acid, oleic acid 1~10mol of amine are successively added,
Then 1~5mol of diacetyl acetone platinum is dissolved in the obtained mixture containing phenyl ether, and reacted under the conditions of 150 DEG C
40~80min, continue to be warming up to 180~200 DEG C, according to praseodynium iron：Diacetyl acetone platinum=1:1.2~1.4 rub
You add praseodynium iron at ratio, keep constant temperature to continue 50~70min of reaction and obtain the Fe3O4/ Pt magnetic nanoparticles.
Thus, preparation method is simply easily achieved, and yield is high.
According to an embodiment of the invention, Fe is formed3O4/SiO2Magnetic nanoparticle can be carried out by following steps：Make to contain
There are the solution of ferrous ion and iron ion and the mixed reaction of ammoniacal liquor, obtain ferroferric oxide magnetic nanoparticle, make four oxidation
Three ferromagnetic nanoparticles react with the mixture of TMAH and tetraethyl orthosilicate, obtain Fe3O4/SiO2Magnetic is received
Rice grain.Thereby, it is possible to form nucleocapsid protection structure, preparation method is simply easily achieved, and yield is high.
According to some specific embodiments of the present invention, Fe is formed3O4/SiO2Magnetic nanoparticle can pass through following steps
Carry out：It is Fe according to molar ratio2+:Fe3+=1:1.5~2 configurations solution containing ferrous ion and iron ion, control
Bath temperature stirs at 30~90 DEG C, in molar ratio example Fe3+:Ammoniacal liquor=1：4~8 slowly pour into 25 mass % dense ammonia
Water, continue to stir 5~30min of precipitation reaction in water-bath, obtain Fe3O4Magnetic nanoparticle, by the Fe3O4Magnetic Nano
Grain is dissolved in 200ml TMAHs and 10~30min of ultrasonic disperse, according to mass ratio Fe3O4:Tetraethyl orthosilicate=
2.4~7.2:1 adds tetraethyl orthosilicate, and stirring reaction 4~8 hours, obtains the Fe at 25 DEG C3O4/SiO2Magnetic Nano
Grain.Thus, preparation method is simply easily achieved, and yield is high.
According to an embodiment of the invention, after preparing magnetic nanoparticle by above-mentioned steps, can also include to magnetic
The step of property nano particle is post-processed, specific post-processing step is not particularly limited, and those skilled in the art can root
According to needs flexibly selection.In some embodiments of the invention, the reacted reaction solution of final step is moved into 1000ml beakers,
Settle, and washed repeatedly with deionized water 5~7 times under magnetic support, until examining in washing lotion without Cl-And SO4 2-And pH=7 is
Only.Gained magnetic nanoparticle is moved into surface plate, is put into vacuum drying chamber and dries, vacuum is -0.1Mpa, heating temperature
Spend for 30~90 DEG C, drying time is generally 24~48 hours, dried magnetic nanoparticle is ground standby.By
This, free from admixture in magnetic nanoparticle, granularity is small, be easy to subsequently with base load liquid married operation.
S200：Magnetic nanoparticle and K-Na alloy-baseds carrier fluid are mixed.
According to an embodiment of the invention, the mode that magnetic nanoparticle and K-Na alloy-baseds carrier fluid mix is not limited especially
System, those skilled in the art can flexibly select.In some embodiments of the invention, by magnetic nanoparticle and K-Na alloys
The mixing of base load liquid includes：Under anhydrous and oxygen-free, argon gas protection environment, by the magnetic nanoparticle and the K-Na alloys base load
Liquid is immersed in paraffin oil, and water-bath is heated slowly to 30~70 DEG C, and gentle, intermittence is stirred until homogeneous mixing, is removed upper liquid, is obtained
To the magnetic liquid.Thus, preparation method is simply easily achieved, and yield is high, low for equipment requirements.
According to an embodiment of the invention, S200 further comprises：Under anhydrous and oxygen-free, argon gas protection environment, according to Fe3O4/
Au、Fe3O4/Ag、Fe3O4/Pt、Fe3O4/SiO2The quality proportioning of magnetic nanoparticle and K-Na alloy-based carrier fluids is respectively 0.56
~5.59:1,0.4~4.03:1,0.59~5.94:1,0.26~2.62:1 weighs magnetic nanoparticle and K-Na alloy base loads
Liquid is standby.Corresponding magnetic nanoparticle and K-Na alloy-baseds carrier fluid are immersed in paraffin oil, water-bath is heated slowly to 30~70
At DEG C, the two gentle, intermittence is stirred by 40~120min using glass bar, after the mixing of the two substantially uniformity, removes upper strata
Liquid produces K-Na alloy based magnetic liquids.Thus, preparation method is simply easily achieved, and yield is high, low for equipment requirements.
According to an embodiment of the invention, in general magnetic liquid, use temperature range is narrower, and higher or lower temperature
When spending magnetic liquid occur volatilization, freeze or base load liquid and surfactant cracking and cause magnetic liquid fail ask
Topic.And mix magnetic nanoparticle with K-Na alloy-based carrier fluids in the present invention, the magnetic liquid use temperature range of acquisition is wide,
Use demand under particular surroundings can be competent at, the coefficient of heat conduction is high, and good conductivity is corrosion-resistant, can play sealing, cooling simultaneously
With the effect of lubrication, so as to for atomic energy nuclear reactor or other military industry fields, and solve Aero-Space, machinery, chemical industry,
The problems such as long-standing sealing of the industry visual plant such as pharmacy, biology, cooling and lubrication.
Specific embodiment
Embodiment 1
1st, magnetic nanoparticle is formed
(1) Fe is formed3O4/ Au magnetic nanoparticles
It is Fe according to molar ratio2+:Fe3+=1:1.5 configuration Fe2+And Fe3+Solution, control bath temperature stir at 30 DEG C
Mix, in molar ratio example Fe3+:Ammoniacal liquor=1:4 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, water-bath relaying
Continuous stirring precipitation reaction 5min, that is, prepare exposed Fe3O4Magnetic nanoparticle.The Fe that will be prepared3O4It is dissolved in
In 0.1mol/L TMAH, 10min is cleaned using 0.1mol/L sodium citrate, according to Fe3O4:HAuCl4Matter
Amount is than being 1:8 add 1% HAuCl4Solution, then according to mass ratio HAuCl4:NH2OHHCl=1:2.5 add NH2OH·
HCl, reduction reaction 2 hours, produces Fe3O4/ Au magnetic nanoparticles.
(2) Fe is formed3O4/ Ag magnetic nanoparticles
It is Fe according to molar ratio2+:Fe3+=1:1.5 configuration Fe2+And Fe3+Solution, control bath temperature stir at 30 DEG C
Mix, in molar ratio example Fe3+:Ammoniacal liquor=1:4 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, water-bath relaying
Continuous stirring precipitation reaction 5min, that is, prepare exposed Fe3O4Magnetic nanoparticle.The Fe that will be prepared3O4It is dissolved in
In 0.1mol/L TMAH, 10min is cleaned using 0.1mol/L sodium citrate, according to Fe3O4:AgNO3Quality
Than for 1:3.2 add 1% AgNO3Solution, then according to mass ratio AgNO3:NH2OHHCl=1:0.8 adds NH2OH·
HCl, reduction reaction 2 hours, produces Fe3O4/ Ag magnetic nanoparticles.
(3) Fe is formed3O4/ Pt magnetic nanoparticles
In 200ml phenyl ethers, 10mol polyethylene glycol -200, oleic acid 2mol, oleic acid amine 2mol are successively added, then will
Diacetyl acetone platinum 1mol is dissolved in phenyl ether.Said mixture is heated to 150 DEG C of reaction 40min, continues to be warming up to 180
DEG C, according to praseodynium iron：Diacetyl acetone platinum=1:1.2 molar ratio adds praseodynium iron, keep constant temperature after
Continuous reaction 50min.Dark-brown reaction solution is cooled to room temperature, and with ethanol washing precipitate, centrifuges 5min, removes upper liquid.
Sediment is dissolved in toluene and continues to be cleaned with ethanol, is centrifuged, so at least repeatedly 3 times, finally washed, dried i.e. with acetone
Fe can be obtained3O4/ Pt magnetic nanoparticles.
(4) Fe is formed3O4/SiO2Magnetic nanoparticle
It is Fe according to molar ratio2+：Fe3+=1:1.5 configuration Fe2+And Fe3+Solution, control bath temperature stir at 30 DEG C
Mix, in molar ratio example Fe3+:Ammoniacal liquor=1:4 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, water-bath relaying
Continuous stirring precipitation reaction 5min, that is, prepare exposed Fe3O4Magnetic nanoparticle.Magnetic nanoparticle is dissolved in 200ml tetra-
Ultrasonic disperse 10min in ammonium hydroxide, according to mass ratio Fe3O4:Tetraethyl orthosilicate=7.2:1 addition tetraethyl orthosilicate, 25
Stirring reaction 4 hours, produce Fe at DEG C3O4/SiO2Magnetic nanoparticle.
2nd, the post processing of magnetic nanoparticle
The different reacted reaction solutions immigration 1000ml beakers of magnetic nanoparticle final step are prepared by above-mentioned, in magnetic support
Lower sedimentation, and washed repeatedly with deionized water 5 times, until examining in washing lotion without Cl-And SO4 2-And untill pH=7.By gained
Magnetic nanoparticle is moved into surface plate, is put into vacuum drying chamber and is dried, and vacuum is -0.1Mpa, and heating-up temperature is 50 DEG C,
Drying time is generally 24 hours, dried magnetic nanoparticle is ground standby.
3rd, magnetic nanoparticle and K-Na alloy-baseds carrier fluid are mixed
According to Fe3O4/Au、Fe3O4/Ag、Fe3O4/Pt、Fe3O4/SiO2Magnetic nanoparticle and K-Na alloy-based carrier fluids
Quality proportioning is respectively 0.56:1,0.4:1,0.59:1,0.26:1 weighs magnetic nanoparticle and K-Na alloy-based carrier fluids respectively
It is standby.Corresponding magnetic nanoparticle and K-Na alloy-baseds carrier fluid are immersed in paraffin oil, water-bath is heated slowly at 30 DEG C, is adopted
The two gentle, intermittence is stirred into 40min with glass bar, after the mixing of the two substantially uniformity, obtained respectively after removing upper liquid：
Only contain Fe3O4The K-Na alloys based magnetic liquid of/Au magnetic nanoparticles, only contain Fe3O4The K- of/Ag magnetic nanoparticles
Na alloys based magnetic liquid, only contain Fe3O4The K-Na alloys based magnetic liquid of/Pt magnetic nanoparticles, only contain Fe3O4/
SiO2The K-Na alloy based magnetic liquids of magnetic nanoparticle.Aforesaid operations are carried out under anhydrous and oxygen-free, argon gas protection environment.
It is 82Gs, 86Gs, 79Gs and 105Gs corresponding to the magnetic liquid saturation magnetization of above-mentioned acquisition.These magnetic liquids use
Temperature range is -11~785 DEG C, can be competent at use demand under particular surroundings, and the coefficient of heat conduction is high, and good conductivity is corrosion-resistant,
Sealing, cooling and lubrication can be played a part of simultaneously, so as to for atomic energy nuclear reactor or other military industry fields, and solved
Certainly the problems such as the long-standing sealing of the industry visual plant such as Aero-Space, machinery, chemical industry, pharmacy, biology, cooling and lubrication.
Embodiment 2
1st, magnetic nanoparticle is formed
(1) Fe is formed3O4/ Au magnetic nanoparticles
It is Fe according to molar ratio2+:Fe3+=1:1.75 configure Fe2+And Fe3+Solution, control bath temperature stir at 60 DEG C
Mix, in molar ratio example Fe3+:Ammoniacal liquor=1:6 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, water-bath relaying
Continuous stirring precipitation reaction 15min, that is, prepare exposed Fe3O4Magnetic nanoparticle.The Fe that will be prepared3O4It is dissolved in
In 0.1mol/L TMAH, 10min is cleaned using 0.1mol/L sodium citrate, according to Fe3O4:HAuCl4Matter
Amount is than being 1:4 add 1% HAuCl4Solution, then according to mass ratio HAuCl4:NH2OHHCl=1:4 add NH2OH·
HCl, reduction reaction 2 hours, produces Fe3O4/ Au and Fe3O4/ Ag magnetic nanoparticles.
(2) Fe is formed3O4/ Ag magnetic nanoparticles
It is Fe according to molar ratio2+:Fe3+=1:1.75 configure Fe2+And Fe3+Solution, control bath temperature stir at 60 DEG C
Mix, in molar ratio example Fe3+:Ammoniacal liquor=1:6 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, water-bath relaying
Continuous stirring precipitation reaction 15min, that is, prepare exposed Fe3O4Magnetic nanoparticle.The Fe that will be prepared3O4It is dissolved in
In 0.1mol/L TMAH, 10min is cleaned using 0.1mol/L sodium citrate, according to Fe3O4:AgNO3Quality
Than for 1:1.6 add 1% AgNO3Solution, then according to mass ratio AgNO3:NH2OHHCl=1:1.4 add NH2OH·
HCl, reduction reaction 2 hours, produces Fe3O4/ Au and Fe3O4/ Ag magnetic nanoparticles.
(3) Fe is formed3O4/ Pt magnetic nanoparticles
In 200ml phenyl ethers, 15mol polyethylene glycol -200, oleic acid 4mol, oleic acid amine 4mol are successively added, then will
Diacetyl acetone platinum 3mol is dissolved in phenyl ether.Said mixture is heated to 150 DEG C of reaction 60min, continues to be warming up to 190
DEG C, according to praseodynium iron：Diacetyl acetone platinum=1:1.3 molar ratio adds praseodynium iron, keep constant temperature after
Continuous reaction 60min.Dark-brown reaction solution is cooled to room temperature, and with ethanol washing precipitate, centrifuges 5min, removes upper liquid.
Sediment is dissolved in toluene and continues to be cleaned with ethanol, is centrifuged, so at least repeatedly 3 times, finally washed, dried i.e. with acetone
Fe can be obtained3O4/ Pt magnetic nanoparticles.
(4) Fe is formed3O4/SiO2Magnetic nanoparticle
It is Fe according to molar ratio2+:Fe3+=1:1.75 configure Fe2+And Fe3+Solution, control bath temperature stir at 60 DEG C
Mix, in molar ratio example Fe3+:Ammoniacal liquor=1:6 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, water-bath relaying
Continuous stirring precipitation reaction 15min, that is, prepare exposed Fe3O4Magnetic nanoparticle, its TEM figures reference picture 1.By magnetic Nano
Grain dissolution ultrasonic disperse 20min in 200ml TMAHs, according to mass ratio Fe3O4:Tetraethyl orthosilicate=4.1:1
Tetraethyl orthosilicate is added, stirring reaction 6 hours, produces Fe at 25 DEG C3O4/SiO2Magnetic nanoparticle.
2nd, the post processing of magnetic nanoparticle
The different reacted reaction solutions immigration 1000ml beakers of magnetic nanoparticle final step are prepared by above-mentioned, in magnetic support
Lower sedimentation, and washed repeatedly with deionized water 7 times, until examining in washing lotion without Cl-And SO4 2-And untill pH=7.By gained
Magnetic nanoparticle is moved into surface plate, is put into vacuum drying chamber and is dried, and vacuum is -0.1Mpa, and heating-up temperature is 90 DEG C,
Drying time is generally 48 hours, dried magnetic nanoparticle is ground standby.
3rd, magnetic nanoparticle and K-Na alloy-baseds carrier fluid are mixed
According to Fe3O4/Au、Fe3O4/Ag、Fe3O4/Pt、Fe3O4/SiO2Magnetic nanoparticle and K-Na alloy-based carrier fluids
Quality proportioning is respectively 5.59:Isosorbide-5-Nitrae .03:1,5.94:1,2.62:1 weighs magnetic nanoparticle and K-Na alloy-based carrier fluids are standby
With.Corresponding magnetic nanoparticle and K-Na alloy-baseds carrier fluid are immersed in paraffin oil, water-bath is heated slowly at 70 DEG C, is used
The two gentle, intermittence is stirred 120min by glass bar, after the mixing of the two substantially uniformity, is obtained respectively after removing upper liquid：
Only contain Fe3O4The K-Na alloys based magnetic liquid of/Au magnetic nanoparticles, only contain Fe3O4The K- of/Ag magnetic nanoparticles
Na alloys based magnetic liquid, only contain Fe3O4The K-Na alloys based magnetic liquid of/Pt magnetic nanoparticles, only contain Fe3O4/
SiO2The K-Na alloy based magnetic liquids of magnetic nanoparticle.Aforesaid operations are carried out under anhydrous and oxygen-free, argon gas protection environment.
It is 369Gs, 352Gs, 380Gs and 470Gs corresponding to the magnetic liquid saturation magnetization of above-mentioned acquisition, wherein, only contain
Fe3O4/SiO2The magnetization curve of the K-Na alloy based magnetic liquids of magnetic nanoparticle is shown in Fig. 2.These magnetic liquid temperature in use
Scope is wide, can be competent at use demand under particular surroundings, the coefficient of heat conduction is high, and good conductivity is corrosion-resistant, can play simultaneously close
Envelope, cooling and the effect of lubrication, so as to for atomic energy nuclear reactor or other military industry fields, and solve Aero-Space, machine
The problems such as long-standing sealing of the industry visual plant such as tool, chemical industry, pharmacy, biology, cooling and lubrication.
Embodiment 3
1st, magnetic nanoparticle is formed
(1) Fe is formed3O4/ Au magnetic nanoparticles
It is Fe according to molar ratio2+:Fe3+=1:2 configuration Fe2+And Fe3+Solution, control bath temperature stir at 90 DEG C,
Example Fe in molar ratio3+:Ammoniacal liquor=1:8 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, continues to stir in water-bath
Precipitation reaction 30min is mixed, that is, prepares exposed Fe3O4Magnetic nanoparticle.The Fe that will be prepared3O4It is dissolved in 0.1mol/L
TMAH in, using 0.1mol/L sodium citrate clean 10min, according to Fe3O4:HAuCl4Mass ratio is 1:
0.3 adds 1% HAuCl4Solution, then according to mass ratio HAuCl4:NH2OHHCl=1:6 add NH2OHHCl, reduction
Reaction 2 hours, produces Fe3O4/ Au magnetic nanoparticles.
(2) Fe is formed3O4/ Ag magnetic nanoparticles
It is Fe according to molar ratio2+:Fe3+=1:2 configuration Fe2+And Fe3+Solution, control bath temperature stir at 90 DEG C,
Example Fe in molar ratio3+:Ammoniacal liquor=1:8 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, continues to stir in water-bath
Precipitation reaction 30min is mixed, that is, prepares exposed Fe3O4Magnetic nanoparticle.The Fe that will be prepared3O4It is dissolved in 0.1mol/L
TMAH in, using 0.1mol/L sodium citrate clean 10min, according to Fe3O4:AgNO3Mass ratio is 1:
0.1 adds 1% AgNO3Solution, then according to mass ratio AgNO3:NH2OHHCl=1:2 add NH2OHHCl, reduction are anti-
Answer 2 hours, produce Fe3O4/ Ag magnetic nanoparticles.
(3) Fe is formed3O4/ Pt magnetic nanoparticles
In 200ml phenyl ethers, 20mol polyethylene glycol -200, oleic acid 8mol, oleic acid amine 10mol are successively added, then will
Diacetyl acetone platinum 5mol is dissolved in phenyl ether.Said mixture is heated to 150 DEG C of reaction 80min, continues to be warming up to 200
DEG C, according to praseodynium iron：Diacetyl acetone platinum=1:1.4 molar ratio adds praseodynium iron, keep constant temperature after
Continuous reaction 70min.Dark-brown reaction solution is cooled to room temperature, and with ethanol washing precipitate, centrifuges 5min, removes upper liquid.
Sediment is dissolved in toluene and continues to be cleaned with ethanol, is centrifuged, so at least repeatedly 3 times, finally washed, dried i.e. with acetone
Fe can be obtained3O4/ Pt magnetic nanoparticles.
(4) Fe is formed3O4/SiO2Magnetic nanoparticle
It is Fe according to molar ratio2+:Fe3+=1:2 configuration Fe2+And Fe3+Solution, control bath temperature stir at 90 DEG C,
Example Fe in molar ratio3+:Ammoniacal liquor=1:8 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, continues to stir in water-bath
Precipitation reaction 30min is mixed, that is, prepares exposed Fe3O4Magnetic nanoparticle.Magnetic nanoparticle is dissolved in 200ml tetramethyls
Ultrasonic disperse 30min in base ammonium hydroxide, according to mass ratio Fe3O4:Tetraethyl orthosilicate=2.4:1 addition tetraethyl orthosilicate, 25 DEG C
Lower stirring reaction 8 hours, produces Fe3O4/SiO2Magnetic nanoparticle.
2nd, the post processing of magnetic nanoparticle
The different reacted reaction solutions immigration 1000ml beakers of magnetic nanoparticle final step are prepared by above-mentioned, in magnetic support
Lower sedimentation, and washed repeatedly with deionized water 6 times, until examining in washing lotion without Cl-And SO42-And untill pH=7.By gained
Magnetic nanoparticle is moved into surface plate, is put into vacuum drying chamber and is dried, and vacuum is -0.1Mpa, and heating-up temperature is 60 DEG C,
Drying time is generally 30 hours, dried magnetic nanoparticle is ground standby.
3rd, magnetic nanoparticle and K-Na alloy-baseds carrier fluid are mixed
According to Fe3O4/Au、Fe3O4/Ag、Fe3O4/Pt、Fe3O4/SiO2Magnetic nanoparticle and K-Na alloy-based carrier fluids
Quality proportioning is respectively 3.2:1,2.6:Isosorbide-5-Nitrae:1,1.6:1 weighs magnetic nanoparticle and K-Na alloy-based carrier fluids are standby.Will be right
The magnetic nanoparticle and K-Na alloy-baseds carrier fluid answered are immersed in paraffin oil, and water-bath is heated slowly at 50 DEG C, using glass bar
The two gentle, intermittence is stirred into 80min, after the mixing of the two substantially uniformity, obtained respectively：Only contain Fe3O4/ Au magnetic is received
The K-Na alloys based magnetic liquid of rice grain, only contain Fe3O4The K-Na alloys based magnetic liquid of/Ag magnetic nanoparticles, only contain
There is Fe3O4The K-Na alloys based magnetic liquid of/Pt magnetic nanoparticles, only contain Fe3O4/SiO2The K-Na of magnetic nanoparticle is closed
Auri magnetic liquid.Aforesaid operations are carried out under anhydrous and oxygen-free, argon gas protection environment.The magnetic liquid saturation magnetic of above-mentioned acquisition
It is 218Gs, 234Gs, 259Gs and 301Gs to change corresponding to intensity.These magnetic liquid use temperature ranges are wide, can be competent at spy
Use demand under different environment, the coefficient of heat conduction is high, and good conductivity is corrosion-resistant, can play the work of sealing, cooling and lubrication simultaneously
With so as to for atomic energy nuclear reactor or other military industry fields, and solving Aero-Space, machinery, chemical industry, pharmacy, biology
The problems such as sealing long-standing etc. industry visual plant, cooling and lubrication.
Embodiment 4
1st, magnetic nanoparticle is formed
(1) Fe is formed3O4/ Au magnetic nanoparticles
It is Fe according to molar ratio2+:Fe3+=1:1.75 configure Fe2+And Fe3+Solution, control bath temperature stir at 60 DEG C
Mix, in molar ratio example Fe3+:Ammoniacal liquor=1:6 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, water-bath relaying
Continuous stirring precipitation reaction 15min, that is, prepare exposed Fe3O4Magnetic nanoparticle.The Fe that will be prepared3O4It is dissolved in
In 0.1mol/L TMAH, 10min is cleaned using 0.1mol/L sodium citrate, according to Fe3O4:HAuCl4Matter
Amount is than being 1:4 add 1% HAuCl4Solution, then according to mass ratio HAuCl4:NH2OHHCl=1:3.8 add NH2OH·
HCl, reduction reaction 2 hours, produces Fe3O4/ Au magnetic nanoparticles.
(2) Fe is formed3O4/ Ag magnetic nanoparticles
It is Fe according to molar ratio2+:Fe3+=1:1.75 configure Fe2+And Fe3+Solution, control bath temperature stir at 60 DEG C
Mix, in molar ratio example Fe3+:Ammoniacal liquor=1:6 slowly pour into 25% concentrated ammonia liquor, and reaction solution immediately becomes black, water-bath relaying
Continuous stirring precipitation reaction 15min, that is, prepare exposed Fe3O4Magnetic nanoparticle.The Fe that will be prepared3O4It is dissolved in
In 0.1mol/L TMAH, 10min is cleaned using 0.1mol/L sodium citrate, according to Fe3O4:AgNO3Quality
Than for 1:1.6 add 1% AgNO3Solution, then according to mass ratio AgNO3:NH2OHHCl=1:1.5 add NH2OH·
HCl, reduction reaction 2 hours, produces Fe3O4/ Ag magnetic nanoparticles.
2nd, the post processing of magnetic nanoparticle
The different reacted reaction solutions immigration 1000ml beakers of magnetic nanoparticle final step are prepared by above-mentioned, in magnetic support
Lower sedimentation, and washed repeatedly with deionized water 6 times, until examining in washing lotion without Cl-And SO42-And untill pH=7.By gained
Magnetic nanoparticle is moved into surface plate, is put into vacuum drying chamber and is dried, and vacuum is -0.1Mpa, and heating-up temperature is 60 DEG C,
Drying time is generally 30 hours, dried magnetic nanoparticle is ground standby.
3rd, magnetic nanoparticle and K-Na alloy-baseds carrier fluid are mixed
According to Fe3O4/ Au and Fe3O4The quality proportioning of/Ag magnetic nanoparticles and K-Na alloy-based carrier fluids is respectively 3.4:
1 and 2.1:1 weighs magnetic nanoparticle and K-Na alloy-based carrier fluids are standby.By Fe3O4/ Au magnetic nanoparticles, Fe3O4/ Ag magnetic
Property nano particle, K-Na alloy-based carrier fluid threes are immersed in paraffin oil jointly, and water-bath is heated slowly at 50 DEG C, using glass bar
The two gentle, intermittence is stirred into 80min, after the mixing of three's substantially uniformity, acquisition contains Fe simultaneously3O4/ Au magnetic Nanos
Grain and Fe3O4The K-Na alloy based magnetic liquids of/Ag magnetic nanoparticles.Aforesaid operations are in anhydrous and oxygen-free, argon gas protection environment
Lower progress.The magnetic liquid saturation magnetization of acquisition is 206Gs.Gained magnetic liquid use temperature range is wide, can be competent at
Use demand under particular surroundings, the coefficient of heat conduction is high, and good conductivity is corrosion-resistant, can play sealing, cooling and lubrication simultaneously
Effect, so as to for atomic energy nuclear reactor or other military industry fields, and solve Aero-Space, machinery, chemical industry, pharmacy, life
The problems such as long-standing sealing of the industry visual plant such as thing, cooling and lubrication.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description
Point is contained at least one embodiment or example of the present invention.In this manual, to the schematic representation of above-mentioned term not
Identical embodiment or example must be directed to.Moreover, specific features, structure, material or the feature of description can be with office
Combined in an appropriate manner in one or more embodiments or example.In addition, in the case of not conflicting, the skill of this area
Art personnel can be tied the different embodiments or example and the feature of different embodiments or example described in this specification
Close and combine.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changed, replacing and modification.
Claims (9)
- A kind of 1. magnetic liquid, it is characterised in that including：Magnetic nanoparticle, the magnetic nanoparticle have inner core and shell, and the shell is coated on the inner core at least On a part of outer surface, the material for forming the inner core is Fe3O4Magnetic nanoparticle, formed the shell material be selected from Au, Ag, Pt and SiO2At least one of；K-Na alloy-based carrier fluids.
- 2. magnetic liquid according to claim 1, it is characterised in that the magnetic nanoparticle is selected from Fe3O4/ Au magnetic Property nano particle, Fe3O4/ Ag magnetic nanoparticles, Fe3O4/ Pt magnetic nanoparticles and Fe3O4/SiO2In magnetic nanoparticle At least one.
- 3. magnetic liquid according to claim 2, it is characterised in that the Fe3O4/ Au magnetic nanoparticles, Fe3O4/Ag Magnetic nanoparticle, Fe3O4/ Pt magnetic nanoparticles and Fe3O4/SiO2Magnetic nanoparticle and the K-Na alloy-baseds carrier fluid Mass ratio is respectively 0.56~5.59:1,0.4~4.03:1,0.59~5.94:1 and 0.26~2.62:1.
- 4. according to the magnetic liquid any one of claim 1-3, it is characterised in that the temperature in use of the magnetic liquid For -11~785 DEG C.
- 5. according to the magnetic liquid any one of claim 1-3, it is characterised in that the saturated magnetization of the magnetic liquid Intensity is 1~470Gs.
- A kind of 6. method for preparing the magnetic liquid any one of claim 1-5, it is characterised in that including：Magnetic nanoparticle is formed, the magnetic nanoparticle has inner core and shell, and the shell is coated on the inner core On at least a portion outer surface, the material for forming the inner core is Fe3O4Magnetic nanoparticle, the material for forming the shell are Selected from Au, Ag, Pt and SiO2At least one of；The magnetic nanoparticle and K-Na alloy-baseds carrier fluid are mixed.
- 7. according to the method for claim 6, it is characterised in that it is described formation magnetic nanoparticle include following (1), (2), And at least one of (4) (3)：(1) make the solution containing ferrous ion and iron ion and the mixed reaction of ammoniacal liquor, obtain ferroferric oxide magnetic nanoparticle, make The ferroferric oxide magnetic nanoparticle successively with HAuCl4And NH2OHHCl reacts, and obtains Fe3O4/ Au magnetic Nanos Grain；(2) make the solution containing ferrous ion and iron ion and the mixed reaction of ammoniacal liquor, obtain ferroferric oxide magnetic nanoparticle, make The ferroferric oxide magnetic nanoparticle successively with AgNO3And NH2OHHCl reacts, and obtains Fe3O4/ Ag magnetic Nanos Grain；(3) mixture of diacetyl acetone platinum and phenyl ether, polyethylene glycol, oleic acid and oleic acid amine is reacted, and will be resulting Product reacts with praseodynium iron, obtains Fe3O4/ Pt magnetic nanoparticles；(4) make the solution containing ferrous ion and iron ion and the mixed reaction of ammoniacal liquor, obtain ferroferric oxide magnetic nanoparticle, make The ferroferric oxide magnetic nanoparticle reacts with the mixture of TMAH and tetraethyl orthosilicate, obtains Fe3O4/ SiO2Magnetic nanoparticle.
- 8. according to the method for claim 7, it is characterised in that (1) further comprises：It is Fe according to molar ratio2+:Fe3+=1:1.5~2 configurations solution containing ferrous ion and iron ion, controls water Bath temperature stirs at 30~90 DEG C, in molar ratio example Fe3+:Ammoniacal liquor=1:4~8 slowly pour into 25 mass % concentrated ammonia liquor, Continue to stir 5~30min of precipitation reaction in water-bath, obtain Fe3O4Magnetic nanoparticle, by the Fe3O4Magnetic nanoparticle is molten Solution cleans 10min in 0.1mol/L TMAH, using 0.1mol/L sodium citrate, according to the Fe3O4Magnetic Property nano particle:HAuCl4Mass ratio is 1:8~0.3 add 1 mass % HAuCl4Solution, then according to mass ratio HAuCl4: NH2OHHCl=1:2.5~6 add NH2OHHCl, reduction reaction 2 hours, produces the Fe3O4/ Au magnetic nanoparticles；(2) further comprise：It is Fe according to molar ratio2+:Fe3+=1:1.5~2 configurations solution containing ferrous ion and iron ion, controls water Bath temperature stirs at 30~90 DEG C, in molar ratio example iron ion:Ammoniacal liquor=1:4~8 slowly pour into 25 mass % dense ammonia Water, continue to stir 5~30min of precipitation reaction in water-bath, obtain Fe3O4Magnetic nanoparticle, by the Fe3O4Magnetic Nano Grain is dissolved in 0.1mol/L TMAH, 10min is cleaned using 0.1mol/L sodium citrate, according to described Fe3O4Magnetic nanoparticle:AgNO3Mass ratio is 1:3.2~0.1 add 1 mass % AgNO3Solution, then according to mass ratio AgNO3:NH2OHHCl=1:0.8~2 adds NH2OHHCl, reduction reaction 2 hours, produces the Fe3O4/ Ag magnetic Nanos Particle；(3) further comprise：In 200ml phenyl ethers, 10~20mol polyethylene glycol -200,1~8mol of oleic acid, oleic acid 1~10mol of amine are successively added, Then 1~5mol of diacetyl acetone platinum is dissolved in the obtained mixture containing phenyl ether, and reacted under the conditions of 150 DEG C 40~80min, continue to be warming up to 180~200 DEG C, according to praseodynium iron：Diacetyl acetone platinum=1:1.2~1.4 rub You add praseodynium iron at ratio, keep constant temperature to continue 50~70min of reaction and obtain the Fe3O4/ Pt magnetic nanoparticles；(4) further comprise：It is Fe according to molar ratio2+：Fe3+=1：1.5~2 configurations solution containing ferrous ion and iron ion, controls water Bath temperature stirs at 30~90 DEG C, in molar ratio example Fe3+：Ammoniacal liquor=1：4~8 slowly pour into 25 mass % concentrated ammonia liquor, Continue to stir 5~30min of precipitation reaction in water-bath, obtain Fe3O4Magnetic nanoparticle, by the Fe3O4Magnetic nanoparticle is molten Solution is in 200ml TMAHs and 10~30min of ultrasonic disperse, according to mass ratio Fe3O4:Tetraethyl orthosilicate=2.4~ 7.2:1 adds tetraethyl orthosilicate, and stirring reaction 4~8 hours, obtains the Fe at 25 DEG C3O4/SiO2Magnetic nanoparticle.
- 9. according to the method for claim 6, it is characterised in that described by the magnetic nanoparticle and K-Na alloy base loads Liquid mixing includes：Under anhydrous and oxygen-free, argon gas protection environment, the magnetic nanoparticle and the K-Na alloy-baseds carrier fluid are immersed into paraffin In oil, water-bath is heated slowly to 30~70 DEG C, and gentle, intermittence is stirred until homogeneous mixing, removes upper liquid, obtains the magnetic Liquid.
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| CN101789296A (en) * | 2010-02-08 | 2010-07-28 | 北京交通大学 | Preparation method of gold-covered nano magnetic particle used for preparing magnetic liquid |
| CN105754095A (en) * | 2016-03-18 | 2016-07-13 | 河南大学 | Preparation method and application of Fe3O4@PPy@Au magnetic composite microspheres |
| CN106298145A (en) * | 2016-09-23 | 2017-01-04 | 北京交通大学 | A kind of preparation method of the sodium-potassium eutectic based magnetic liquid with conducting function |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101789296A (en) * | 2010-02-08 | 2010-07-28 | 北京交通大学 | Preparation method of gold-covered nano magnetic particle used for preparing magnetic liquid |
| CN105754095A (en) * | 2016-03-18 | 2016-07-13 | 河南大学 | Preparation method and application of Fe3O4@PPy@Au magnetic composite microspheres |
| CN106298145A (en) * | 2016-09-23 | 2017-01-04 | 北京交通大学 | A kind of preparation method of the sodium-potassium eutectic based magnetic liquid with conducting function |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113096906A (en) * | 2021-03-24 | 2021-07-09 | 华南理工大学 | FeSiCr alloy magnetic powder with double coating layers and preparation method thereof, magnetic powder core and preparation method thereof |
| CN113096906B (en) * | 2021-03-24 | 2022-11-18 | 华南理工大学 | FeSiCr alloy magnetic powder with double coating layers and preparation method thereof, magnetic powder core and preparation method thereof |
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