CN103310939B - A kind of plasma helps magnetic liquid and preparation method thereof - Google Patents
A kind of plasma helps magnetic liquid and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of plasma and help NiMnGa/Fe
2o
3magnetic liquid and preparation method thereof, belongs to nano magnetic material field.The method that using plasma is assisted in preparation process, preparation NiMnGa/Fe
2o
3magnetic liquid.Because NiMnGa alloy has higher saturation magnetization and good stability, thus Fe can be increased
2o
3the saturation magnetization of magnetic liquid and stability.The method that using plasma is assisted in preparation process obviously can shorten manufacturing cycle, reduces energy waste, cost-saving.
Description
Technical field
The invention belongs to nano-magnetic fluid and preparation field thereof, particularly a kind of plasma helps magnetic liquid and preparation method and application.
Background technology
Magnetic liquid is a kind of novel liquid functional material, and it is coated by means of surfactant by magnetic-particle, be highly dispersed in stable " solid-liquid " two-phase colloidal solution of the one formed in base load liquid.It had both had the magnetic of solid material, had again the mobility of liquid.Its microstructure forms primarily of three parts: i.e. magnetic-particle, base load liquid and surfactant.
At present, the emphasis of magnetic liquid research in the world selects which kind of magnetic particle and surfactant, and the base oil of blindly dating with surfactant, and to obtain, magnetic property is high, the magnetic liquid of good stability, meets the application of special dimension.Therefore, high saturation and magnetic intensity (M
s) and chemical stability be evaluate the important indicator of magnetic liquid performance.And these two performances are mainly determined by the volume fraction of the characteristic and shared magnetic liquid thereof that form magnetic liquid magnetic particle.In magnetic liquid, magnetic particle generally has iron oxygen type (Fe
30
4, γ-Fe
20
3deng), metal mold (Co, Ni etc.), iron-nitride (Fe
3n etc.) etc.Because ferrite-type magnetic liquid has good stability, become domestic and international application magnetic liquid the most widely.But its shortcoming is M
slower, generally at 0.02 ~ 0.03T, the highlyest only can reach 0.06T, thus limit its range of application.Although the M of metal mold magnetic liquid
shigher, but chemical stability is poor, also makes it apply and is restricted.The iron-nitride magnetic liquid developed in recent years has than ferrite-type and the higher M of metal mold magnetic liquid
sbut the preparation process of magnetic liquid of nitriding iron is more complicated, and magnetic particle not easily detects, stability is not fine.
Magnetically driven shape memory alloy is held concurrently high response frequency and the large feature exporting strain, is subject to extensive concern in recent years.Find that Magnetic driving shape-memory material mainly comprises at present: Ni-Mn-Ga (Al) Ni-Fe-Ga, Fe-Pd (Pt) Co-Ni-Ga (Al) and Ni-Mn-X (x=In, Sn, Sb) etc.Wherein, Ni-Mn-Ga alloy is the magnetically driven shape memory alloy found the earliest.NiMnGa alloy particle has high saturation magnetization and Curie temperature, and the magnetic-field-induced strain being about 10% can be produced, also be the magnetically driven shape memory alloy having application potential most, under normal temperature, nano particle not only keeps the performance of block materials, and has good stability.
Therefore, there is high saturation and magnetic intensity and good stability and there is the focus always received publicity compared with a kind of novel nano magnetic liquid magnetic liquid of high-curie temperature.
Summary of the invention
The object of this invention is to provide a kind of higher magnetization and the two particle magnetic liquid of good stability, plasma helps NiMnGa/Fe
2o
3magnetic liquid and preparation method thereof, this nano-magnetic fluid has comparatively high-curie temperature, is a kind of novel nano magnetic liquid.The magnetic liquid of the present invention method that using plasma is assisted in preparation process, its manufacturing cycle is short, and energy resource consumption is low, cost-saving.
Magnetic liquid of the present invention, its component is: NiMnGa particle, Fe
2o
3particle, polybutylene-based succimide TEPA surfactant and oleic acid; Wherein NiMnGa/Fe
2o
3two particle magnetic alloy particle, particle profile is spherical substantially, and diameter is 100-400nm;
Wherein in NiMnGa particle, the mol ratio of Ni:Mn:Ga is that 5.5-4.5:3.5-2.5:1-3, NiMnGa particle powder diameter is about 300-600nm;
NiMnGa particle: Fe
2o
3particle: polybutylene-based succimide TEPA surfactant: the mass ratio of oleic acid is 1.0-1.5:9-11:1.2-1.7:0.8-1.2.
Magnetic liquid of the present invention, its preparation method is:
1, the preparation of NiMnGa alloy nano particle: adopt arc melting method to be prepared into NiMnGa alloy pig high purity N i, Mn, Ga simple substance, wherein the mol ratio of Ni:Mn:Ga is 5.5-4.5:3.5-2.5:1-3, adopts the method for mechanical ball milling to prepare NiMnGa particle powder diameter about 300-600nm;
2, NiMnGa/Fe
2o
3the preparation of two particle magnetic liquid:
(1) take polybutylene-based succimide TEPA surfactant and oleic acid, mixing, then adds the ultrasonic process of NiMnGa alloyed powder, NiMnGa particle: Fe
2o
3particle: polybutylene-based succimide TEPA surfactant: the mass ratio of oleic acid is 1.0-1.5:9-11:1.2-1.7:0.8-1.2;
(2) ultrasonic good solution is injected in reactor, and inject rapidly carbonyl iron solution in reactor, input nitrogen and argon gas in reactor, argon gas: the flow-rate ratio 4:1 of nitrogen, the carbonyl iron solution added and the mass ratio of NiMnGa particle are 1.0-1.5:22-27;
(3) when being preheated to 130-140 DEG C to reactor, closing and help thermal, device for cooling (0 DEG C) in opening, whole circulation needs time 3-5min; Connection helps thermal, device for cooling in closing, alternating-current pulse high voltage source is connect at electrode interface place, in alternating electric field region, plasma discharge process is carried out to ammonia, carbonyl iron liquid, its pulse frequency regulation and control 63.5-68KHz, regulating and controlling voltage to 10-12kV, operating current 200-400mA, in adjustment reactor, the speed of blender is 170-210rad/min, starts next circulation;
(4) repetitive cycling, totally ten times, approximately runs 120-140min, whole plasma body cooperative synthesis of nano NiMnGa/Fe
2o
3be in the circulation frozen water state of cooling in the process of two particle magnetic liquid always;
(5) question response temperature in the kettle is cooled to room temperature, collects black NiMnGa/Fe
2o
3two particle nano-magnetic fluid.
Polybutylene-based succimide TEPA is surfactant (being called for short PBSI).
The invention has the advantages that the magnetic liquid of the saturation magnetization that acquisition is higher and good stability, because NiMnGa alloy has higher saturation magnetization and good non-oxidizability, thus can increase Fe
2o
3the saturation magnetization of magnetic liquid and stability.The superiority of adopting in this way is that experimental procedure is not loaded down with trivial details, and one-step synthesis obtains product, and the reaction time is short, is easy to scale.Specifically, at Ar and N
2plasma atmosphere under, make the reaction of liquid iron pentacarbonyl, Ni-Mn-Ga particle, surfactant PBSI and oil-base fluid, reaction terminates just to obtain product, and the method overcomes the requirements such as the sealing of the high temperature resistant and reactor of experimental provision.
Accompanying drawing explanation
Fig. 1 plasma assists to prepare liquid nano device, and 1 helps thermal, 2 blenders, 3 electrodes, 4 quartzy umbrellas, device for cooling in 5,6 material injecting devices, 7 cooling devices, 8 electrode interfaces, 9 Inlet and outlet water interfaces, 10 transmission devices, 11 numerical-control motors, 12 turnover gas interfaces, 13 lowering or hoisting gears, 14 micromatic settings, 15 bearing plate adjusting devices, 16 quartz reaction stills, 17 transducers;
Fig. 2 NiMnGa/Fe
2o
3the XRD collection of illustrative plates of two particle magnetic liquid;
Fig. 3 NiMnGa/Fe
2o
3the TEM collection of illustrative plates of two particle magnetic liquid;
Fig. 4 NiMnGa/Fe
2o
3two particle magnetic liquid builds crest state under magnetic fields.
Embodiment
Following examples explains content of the present invention further, but not in order to limit the present invention
Embodiment 1
1, the preparation of NiMnGa alloy particle:
Get the electrolytic nickel (196.4 grams) that purity is 99.99%, the electrolytic manganese (110.3 grams) of 99.95%, the gallium of 99.99% is raw material (93.4g gram), adopts non-consumable arc furnace under the protective atmosphere of argon gas, prepare the Ni-Mn-Ga alloy sample of 400 grams.Before melting, employing mechanical pump, molecular pump are evacuated down to 5 × 10
-3pa, then be filled with high-purity argon gas to 2 × 10
-2pa, starts melting.In order to ensure the uniformity of ingot chemistry, each sample upset melting four times and in addition magnetic stir, then by melted button ingot casting refuse, inhale with the device of water-cooled copper crucible bottom the bar samples casting Φ 10mm × 75mm, treat that its cooling is taken out.Test material removes surface impurity through mechanical polishing, is 10 with enclosing vacuum degree after acetone cleaning
-1in the quartz ampoule of Pa, under 1273K/5h condition, carry out homogenizing annealing process, and to obtain the high degree of order in water of quenching.Then adopting the method for mechanical ball milling to prepare Ni-Mn-Ga particle powder diameter is 400nm;
2, NiMnGa/Fe
2o
3the preparation of two particle magnetic liquid:
(1) ultrasonic process:
Weigh polybutylene-based 6.3 grams, succimide TEPA surfactant and oleic acid 4.2 grams, shake makes it fully mix, then add 4.9 grams of NiMnGa alloyed powders and carry out the ultrasonic process of 10min at SCQ-600 dual-frequency ultrasonic wave washer, supersonic frequency controls at 21000Hz, and power controls at 500W;
(2) toward reactor injection stage:
Fig. 1 is shown in by the structure chart of reactor, injects in reactor 16 by ultrasonic good solution from material injecting device 6, weighs carbonyl iron solution 70ml and injects in reactor 16 from material injecting device 6 rapidly; Be 60sccm by flow-rate ratio 4:1 and nitrogen flow, to be 240sccm input nitrogen and argon gas in reactor 16 from the second turnover gas interface 18 to argon flow amount;
(3) plasma body cooperative active phase:
Connection helps thermal 1, reactor 16 is preheated, the change of real-time detection reaction still 16 inner sensor 17 displays temperature field, when display 130 DEG C, closedown helps thermal 1, device for cooling 5 in opening, carbonyl iron in condensing unit 7 is fallen after rise rapidly in reactor 16, and whole circulation needs time 3min; Connection helps thermal 1, device for cooling 5 in closing, at electrode interface 8, place connects alternating-current pulse high voltage source, in alternating electric field region (electrode 2 and electrode 3 gap), discharge activation is carried out to ammonia, carbonyl iron liquid, its pulse frequency regulation and control 63.5KHz, regulating and controlling voltage to 12kV, operating current 200mA, in adjustment reactor 16, the speed of blender 2 is 170rad/min, starts second circulation;
(4) circulation previous step:
Later repetition second circulation, totally ten times, approximately runs 120-140min, whole plasma body cooperative synthesis of nano NiMnGa/Fe
2o
3be in the circulation frozen water state of cooling in the process of two particle magnetic liquid always;
(5) the cooling bottling stage is shut down:
Using plasma works in coordination with synthesis of nano NiMnGa/Fe
2o
3after two particle magnetic liquid, close AC pulse power supply, help thermal, nitrogen, argon gas, when question response still 16 is cooled to 37 ~ 40 DEG C, open reactor 16, pour black nano magnetic liquid into vial and be built in refrigerating chamber.
Embodiment 2
1, the preparation of NiMnGa alloy particle:
Get the electrolytic nickel (235.7) that purity is 99.99%, the electrolytic manganese (110.3 grams) of 99.95%, the gallium of 99.99% is raw material (140.1g gram), adopts non-consumable arc furnace under the protective atmosphere of argon gas, prepare the Ni-Mn-Ga alloy sample of 486 grams.Before melting, employing mechanical pump, molecular pump are evacuated down to 5 × 10
-3pa, then be filled with high-purity argon gas to 2 × 10
-2pa, starts melting.In order to ensure the uniformity of ingot chemistry, each sample upset melting four times and in addition magnetic stir, then by melted button ingot casting refuse, inhale with the device of water-cooled copper crucible bottom the bar samples casting Φ 10mm × 75mm, treat that its cooling is taken out.Test material removes surface impurity through mechanical polishing, is 10 with enclosing vacuum degree after acetone cleaning
-1in the quartz ampoule of Pa, under 1273K/5h condition, carry out homogenizing annealing process, and to obtain the high degree of order in water of quenching.Then adopting the method for mechanical ball milling to prepare Ni-Mn-Ga particle powder diameter is 300nm;
2, NiMnGa/Fe
2o
3the preparation of two particle magnetic liquid:
(1) ultrasonic process:
Weigh polybutylene-based 5.0 grams, succimide TEPA surfactant and oleic acid 5.0 grams, shake makes it fully mix, then add 6.3 grams of NiMnGa alloyed powders and carry out the ultrasonic process of 10min at SCQ-600 dual-frequency ultrasonic wave washer, supersonic frequency controls at 21000Hz, and power controls at 500W;
(2) toward reactor injection stage:
Fig. 1 is shown in by the structure chart of reactor, injects in reactor 16 by ultrasonic good solution from material injecting device 6, weighs carbonyl iron solution 63ml and injects in reactor 16 from material injecting device 6 rapidly; Be 60sccm by flow-rate ratio 4:1 and nitrogen flow, to be 240sccm input nitrogen and argon gas in reactor 16 from the second turnover gas interface 18 to argon flow amount;
(3) plasma body cooperative active phase:
Connection helps thermal 1, reactor 16 is preheated, the change of real-time detection reaction still 16 inner sensor 17 displays temperature field, when display 130 DEG C, closedown helps thermal 1, device for cooling 5 in opening, carbonyl iron in condensing unit 7 is fallen after rise rapidly in reactor 16, and whole circulation needs time 5min; Connection helps thermal 1, device for cooling 5 in closing, at electrode interface 8, place connects alternating-current pulse high voltage source, in alternating electric field region (electrode 2 and electrode 3 gap), discharge activation is carried out to ammonia, carbonyl iron liquid, its pulse frequency regulation and control 65KHz, regulating and controlling voltage to 10kV, operating current 400mA, in adjustment reactor 16, the speed of blender 2 is 210rad/min, starts second circulation;
(4) circulation previous step:
Later repetition second circulation, totally ten times, approximately runs 140min, whole plasma body cooperative synthesis of nano NiMnGa/Fe
2o
3be in the circulation frozen water state of cooling in the process of two particle magnetic liquid always;
(5) the cooling bottling stage is shut down:
Using plasma works in coordination with synthesis of nano NiMnGa/Fe
2o
3after two particle magnetic liquid, close AC pulse power supply, help thermal, nitrogen, argon gas, when question response still 16 is cooled to 37 DEG C, open reactor 16, pour black nano magnetic liquid into vial and be built in refrigerating chamber.
Embodiment 3
1, the preparation of NiMnGa alloy particle:
Get the electrolytic nickel (157.1 grams) that purity is 99.99%, the electrolytic manganese (73.5 grams) of 99.95%, the gallium of 99.99% is raw material (46.7g gram), adopts non-consumable arc furnace under the protective atmosphere of argon gas, prepare the Ni-Mn-Ga alloy sample of 277 grams.Before melting, employing mechanical pump, molecular pump are evacuated down to 5 × 10
-3pa, then be filled with high-purity argon gas to 2 × 10
-2pa, starts melting.In order to ensure the uniformity of ingot chemistry, each sample upset melting four times and in addition magnetic stir, then by melted button ingot casting refuse, inhale with the device of water-cooled copper crucible bottom the bar samples casting Φ 10mm × 75mm, treat that its cooling is taken out.Test material removes surface impurity through mechanical polishing, is 10 with enclosing vacuum degree after acetone cleaning
-1in the quartz ampoule of Pa, under 1273K/5h condition, carry out homogenizing annealing process, and to obtain the high degree of order in water of quenching.Then adopting the method for mechanical ball milling to prepare Ni-Mn-Ga particle powder diameter is 300-600nm;
2, NiMnGa/Fe
2o
3the preparation of two particle magnetic liquid:
(1) ultrasonic process:
Weigh polybutylene-based 7.1 grams, succimide TEPA surfactant and oleic acid 3.4 grams, shake makes it fully mix, then add 4.2 grams of NiMnGa alloyed powders and carry out the ultrasonic process of 10min at SCQ-600 dual-frequency ultrasonic wave washer, supersonic frequency controls at 21000Hz, and power controls at 500W;
(2) toward reactor injection stage:
Fig. 1 is shown in by the structure chart of reactor, injects in reactor 16 by ultrasonic good solution from material injecting device 6, weighs carbonyl iron solution 78ml and injects in reactor 16 from material injecting device 6 rapidly; Be 60sccm by flow-rate ratio 4:1 and nitrogen flow, to be 240sccm input nitrogen and argon gas in reactor 16 from the second turnover gas interface 18 to argon flow amount;
(3) plasma body cooperative active phase:
Connection helps thermal 1, reactor 16 is preheated, the change of real-time detection reaction still 16 inner sensor 17 displays temperature field, when display 130 DEG C, closedown helps thermal 1, device for cooling 5 in opening, carbonyl iron in condensing unit 7 is fallen after rise rapidly in reactor 16, and whole circulation needs time 3min; Connection helps thermal 1, device for cooling 5 in closing, at electrode interface 8, place connects alternating-current pulse high voltage source, in alternating electric field region (electrode 2 and electrode 3 gap), discharge activation is carried out to ammonia, carbonyl iron liquid, its pulse frequency regulation and control 65KHz, regulating and controlling voltage to 11kV, operating current 400mA, in adjustment reactor 16, the speed of blender 2 is 200rad/min, starts second circulation;
(4) circulation previous step:
Later repetition second circulation, totally ten times, approximately runs 130min, whole plasma body cooperative synthesis of nano NiMnGa/Fe
2o
3be in the circulation frozen water state of cooling in the process of two particle magnetic liquid always;
(5) the cooling bottling stage is shut down:
Using plasma works in coordination with synthesis of nano NiMnGa/Fe
2o
3after two particle magnetic liquid, close AC pulse power supply, help thermal, nitrogen, argon gas, when question response still 16 is cooled to 37 ~ 40 DEG C, open reactor 16, pour black nano magnetic liquid into vial and be built in refrigerating chamber.
Embodiment 4
NiMnGa/Fe
2o
3the institutional framework of two particle magnetic liquid
Utilize 12 kilowatts, Rigaku motor to turn target X-ray diffractometer Rigaku-D/max-rB alloy sample and carry out diffraction analysis, experimental condition is as follows; Cu target K
adiffraction, tube voltage 50kV, tube current 50mA, sweep speed 2/min, λ
k α=0.15418nm.Due to Ni-Mn-Ga alloy standard X-ray diffraction spectrum also not include by ASTM standard card, in the crystal structure list of references of therefore alloy, the existing X-ray diffraction spectrum of Ni-Mn-Ga alloy carries out correlation calibration, determine that the Ni-Mn-Ga alloy in alloy is 5M martensitic crystalline structure, Fe
2o
3alloy is demarcated with reference to PDF card 02-1047.By analyzing in known magnetic liquid containing NiMnGa/Fe
2o
3two particle, and obtain alloy particle in conjunction with Scherrer formula
Diameter 300-400nm.See Fig. 2.
Embodiment 5
By the NiMnGa/Fe of preparation
2o
3magnetic liquid, after room temperature places 60 days, adopts gasoline to dilute with 1:10000, under transmission electron microscope (JEM-2000EX) observes after making sample by TEM sample preparation specification.Visible, in sample, particle profile is spherical substantially and is uniformly dispersed, and narrower particle size distribution, the average diameter of particle is 100-400nm, sees Fig. 3.
Embodiment 6
NiMnGa/Fe
2o
3the magnetic property of two particle magnetic liquid
After major part metal reaches nanometer scale, because skin effect and the light absorbing ability of small-size effect strengthen, size is less, and light absorbing ability is stronger, so the color of magnetic liquid is generally black, crineous.Nano magnetic particle belongs to single domain particulate, is dispersed in base load liquid.When the effect without external magnetic field, magnetic-particle makes its magnetic moment arbitrary orientation due to Blang's warm-up movement, and magnetic is cancelled out each other, and entirety does not externally show magnetic; Under the effect of outside magnetic field, magnetic-particle is geomagnetic into magnetic dipole, and magnetic moment trends towards the direction of external magnetic field, and in catenation between particle.Along with the increase of magnetic field intensity, grain spacing diminishes, and also becomes tight between chain and chain.After removing external magnetic field, magnetic-particle returns to disordered state again.Therefore, magnetic liquid is under magnetic field force, gravity and surface tension comprehensive function, and its surface there will be the spike of ridges and peaks shape, along with the change spike number of magnetic field intensity and distance also can change accordingly, causes liquid level can become unstable.Can design different magnetic circuits, magnetic liquid just can present different states under its effect, sees Fig. 4.
Claims (4)
1. plasma helps a magnetic liquid, it is characterized in that it contains NiMnGa particle, Fe
2o
3particle, polybutylene-based succimide TEPA surfactant and oleic acid, wherein NiMnGa/Fe
2o
3two particle magnetic alloy particle, particle profile is spherical, and diameter is 100-400nm.
2. plasma as claimed in claim 1 helps magnetic liquid, it is characterized in that: NiMnGa particle: Fe
2o
3particle: polybutylene-based succimide TEPA surfactant: the mass ratio of oleic acid is 1.0-1.5:9-11:1.2-1.7:0.8-1.2.
3. plasma as claimed in claim 1 helps magnetic liquid, it is characterized in that: in NiMnGa particle, the mol ratio of Ni:Mn:Ga is 5.5-4.5:3.5-2.5:1-3, NiMnGa particle powder diameter is 300-600nm.
4. a plasma according to claim 1 helps magnetic liquid preparation method as follows:
(1) preparation of NiMnGa alloy nano particle: adopt arc melting method to be prepared into NiMnGa alloy pig high purity N i, Mn, Ga simple substance, wherein the mol ratio of Ni:Mn:Ga is 5.5-4.5:3.5-2.5:1-3, and adopting the method for mechanical ball milling to prepare NiMnGa particle powder diameter is 300-600nm;
(2) NiMnGa/Fe
2o
3the preparation of two particle magnetic liquid:
1) polybutylene-based succimide TEPA surfactant and oleic acid is taken, mixing, then the ultrasonic process of NiMnGa alloyed powder is added, NiMnGa particle: carbonyl iron solution: polybutylene-based succimide TEPA surfactant: the mass ratio of oleic acid is 1.0-1.5:9-11:1.2-1.7:0.8-1.2;
2) ultrasonic good solution is injected in reactor, and inject rapidly carbonyl iron solution in reactor, input nitrogen and argon gas in reactor, argon gas: the flow-rate ratio 4:1 of nitrogen, the carbonyl iron solution added and the mass ratio of NiMnGa particle are 1.0-1.5:22-27; Described ultrasonic good solution is the mixed solution of NiMnGa particle, polybutylene-based succimide TEPA surfactant and oleic acid;
3) when being preheated to 130-140 DEG C to reactor, closing and help thermal, device for cooling in opening, namely 0 DEG C, whole circulation needs time 3-5min; Connection helps thermal, device for cooling in closing, alternating-current pulse high voltage source is connect at electrode interface place, in alternating electric field region, plasma discharge process is carried out to ammonia, carbonyl iron liquid, its pulse frequency regulation and control 63.5-68KHz, regulating and controlling voltage to 10-12kV, operating current 200-400mA, in adjustment reactor, the speed of blender is 170-210rad/min, starts next circulation;
4) repetitive cycling, totally ten times, runs 120-140min, whole plasma body cooperative synthesis of nano NiMnGa/Fe
2o
3be in the circulation frozen water state of cooling in the process of two particle magnetic liquid always;
5) question response temperature in the kettle is cooled to room temperature, obtains NiMnGa/Fe
2o
3two particle nano-magnetic fluid.
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JPH01107502A (en) * | 1987-10-20 | 1989-04-25 | Noboru Ichinose | Manufacture of magnetic fluid |
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