CN109243748B - Double-dispersion magnetorheological fluid and preparation method thereof - Google Patents
Double-dispersion magnetorheological fluid and preparation method thereof Download PDFInfo
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- CN109243748B CN109243748B CN201811185919.7A CN201811185919A CN109243748B CN 109243748 B CN109243748 B CN 109243748B CN 201811185919 A CN201811185919 A CN 201811185919A CN 109243748 B CN109243748 B CN 109243748B
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- 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
- H01F1/447—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids characterised by magnetoviscosity, e.g. magnetorheological, magnetothixotropic, magnetodilatant liquids
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- 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
Abstract
A double-dispersion magnetorheological fluid and a preparation method thereof belong to the technical field of intelligent materials and magnetic materials. The invention adds a small amount of nano-scale magnetic Fe into micron-scale carbonyl iron powder3O4Particles, and gelatin and multi-wall carbon nano-tubes are adopted to wrap carbonyl iron powder and Fe3O4Preparing a double-dispersion magnetorheological fluid as a dispersion phase; the preparation process comprises four steps of coating gelatin, acidifying the multi-walled carbon nano-tube, crosslinking the multi-walled carbon nano-tube and synthesizing the magnetorheological fluid. The invention not only can obviously improve the sedimentation stability of the magnetorheological fluid, but also can enhance the magnetism and rheological property of the magnetorheological fluid, and in addition, the preparation method has simple preparation process, convenient operation and low cost, is suitable for batch production, and can be widely applied to the industrial fields of aerospace, vehicles, machinery and the like.
Description
Technical Field
The invention belongs to the technical field of intelligent materials and magnetic materials, and particularly relates to double-dispersion magnetorheological fluid and a preparation method thereof.
Background
The magnetic rheological liquid is a new type intelligent materialWhen a magnetic field is applied, the Newtonian liquid shows good flowing, but under the action of the external magnetic field, the Newtonian liquid shows the mechanical property similar to solid, but becomes the liquid which can flow once the magnetic field is removed. Therefore, the magnetorheological fluid has the characteristics of rapidness, reversibility and easiness in control, so that the magnetorheological fluid has a very wide application prospect in the fields of aerospace, vehicles, machinery and the like. However, the density of the magnetic particles in the magnetorheological fluid is generally 7-8 g/cm3And the density of the magnetic particles is 7-8 times of that of the carrier liquid, so that the magnetic particles are dispersed in the carrier liquid and are easy to settle, and the rheological property of the magnetorheological fluid is seriously influenced. At present, the common approaches for improving the settleability of the magnetorheological fluid include surface modification of magnetic particles, reduction of the particle size of the magnetic particles, increase of the viscosity of carrier fluid, addition of nano particles and the like. In conventional double-dispersion magnetorheological fluids, Fe3O4At higher temperature, it is easily oxidized into α -Fe2O3Thereby losing magnetism and influencing the performance of the magnetorheological fluid.
Disclosure of Invention
The invention aims to provide a double-dispersion magnetorheological fluid and a preparation method thereof. The double-dispersion magnetorheological fluid aims at obtaining the magnetorheological fluid with good stability, magnetism and rheological property, and micron-sized carbonyl iron powder and nanometer-sized Fe coated by gelatin and multi-walled carbon nano tubes are selected3O4Mixing the microparticles as a dispersed phase; the preparation method of the double-dispersion magnetorheological fluid has the advantages of simple preparation process, convenience in operation and low cost, and is suitable for batch production.
The purpose of the invention is realized as follows:
a double-dispersion magnetorheological fluid comprises carbonyl iron powder and magnetic Fe3O4Carrier liquid, gelatin, multi-walled carbon nanotubes, a stabilizer, a dispersant and a surfactant; the mass fraction of the carbonyl iron powder is more than 98 percent; the magnetic Fe3O4Is more than 80 percent; the mass fraction of the carrier liquid is 20-30%; the multi-wall carbon nano tube accounts for 10 to 15 percent; the mass fraction of the stabilizer is 3-4%; the mass fraction of the dispersant is 1-3%; the mass of the surfactantThe fraction is 1 to 3 percent.
The average grain diameter of the carbonyl iron powder is 3.5 mu m, and the density is 7.9g/cm3。
The magnetic Fe3O4Has an average particle size of 20 nm.
The carrier fluid is a polyolefin synthetic oil.
The gelatin is a coating agent, and can improve the agglomeration and sedimentation performance of magnetic particles.
The multi-walled carbon nano-tube is a cross-linking agent, and can improve the rheological property of the magnetic particles.
The stabilizer is sodium chloride.
The dispersant is oleic acid.
The surfactant is polyethylene glycol.
A preparation method of a double-dispersion magnetorheological fluid comprises the following steps:
step 2, acidification of the multi-walled carbon nanotube: mixing nitric acid and sulfuric acid according to a molar ratio of 3:1 to prepare a strong acid mixed solution; adding the multi-walled carbon nanotube into the mixed solution, heating to 55-65 ℃, and performing ultrasonic irradiation for 12 hours to obtain a strong acid acidified multi-walled carbon nanotube solution;
step 3, crosslinking of the multi-wall carbon nano-tubes: adding the magnetic particles obtained in the step (1) into the solution prepared in the step (2) for crosslinking reaction, performing ultrasonic oscillation to crosslink the multi-walled carbon nanotubes on the surfaces of the magnetic particles, separating the coated magnetic particles under the action of a magnetic field, repeatedly washing with distilled water, and drying;
step 4, synthesis of magnetorheological fluid: and respectively adding the magnetic particles subjected to surface treatment, graphite and polyethylene glycol into the polyolefin synthetic oil, placing the mixture in a water bath environment for heating, starting a magnetic stirrer for stirring, wherein the stirring speed is not too high or too low, and the stirring speed is preferably proper to generate tiny vortexes on the liquid level in a beaker until the uniform double-dispersion magnetorheological fluid is obtained.
In the step 1, the water bath heating temperature is set to be 45-55 ℃, and the time is set to be 30min, so that the gelatin is completely dissolved; the ultrasonic oscillation time is 5-7 h.
In the step 3, the ultrasonic oscillation time is 10-12 h.
In the step 4, the water bath heating temperature is set to be 50-60 ℃, and the time is set to be 50-60 min.
The invention has the beneficial effects that:
(1) the invention relates to a double-dispersion magnetorheological fluid, which is prepared by adopting gelatin and multi-walled carbon nano-tube coated micron-sized carbonyl iron powder and nano-sized Fe3O4The mixed particles are used as a dispersion phase, so that the sedimentation stability of the magnetorheological fluid is improved;
(2) the invention relates to a double-dispersion magnetorheological fluid, which is prepared from magnetic nano particles Fe3O4The magnetic iron-based composite material has superparamagnetism, can be magnetized under the action of a magnetic field, and is filled in gaps formed by long chains of micron-sized carbonyl iron particles, so that the magnetic and rheological effects can be enhanced;
(3) the invention discloses a preparation method of double-dispersion magnetorheological fluid, and particularly relates to four steps of gelatin coating, multi-walled carbon nanotube acidification, multi-walled carbon nanotube crosslinking and magnetorheological fluid synthesis.
Drawings
FIG. 1 is a shear stress variation curve with shear rate of a double-dispersion magnetorheological fluid prepared in example 1 of the present invention and a conventional magnetorheological fluid under different magnetic fields;
FIG. 2 is a graph showing the yield stress of the double-dispersion magnetorheological fluid prepared in example 1 of the present invention and the yield stress of the conventional magnetorheological fluid varying with the intensity of magnetic field;
fig. 3 is a curve of the sedimentation rate of the double-dispersion magnetorheological fluid prepared in the embodiment 1 of the invention and the conventional magnetorheological fluid along with time.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
The preparation method of the invention firstly prepares carbonyl iron powder and magnetic Fe3O4Adding the sodium chloride and the gelatin into a gelatin water solution according to a certain molar ratio, carrying out ultrasonic oscillation, carrying out magnetic separation, washing and drying to obtain the magnetic particles. And then placing the solution in an acidified multi-wall carbon nano tube solution, and carrying out ultrasonic oscillation again, separation, washing and drying. And finally, respectively adding the magnetic particles subjected to surface treatment, graphite and polyethylene glycol into the polyolefin synthetic oil for magnetic stirring to obtain the uniform double-dispersion magnetorheological fluid. The preparation method disclosed by the invention is simple in preparation process and low in cost, and the good coating and crosslinking effects of the gelatin and the multi-walled carbon nano tube are utilized to perform surface modification on the double-dispersion magnetic particles, so that the stability, magnetism and rheological property of the magnetorheological fluid are effectively enhanced, and the magnetorheological fluid has a wide application prospect in the industrial field.
A double-dispersion magnetorheological fluid is characterized by comprising the following raw materials in percentage by mass:
the average grain diameter of the carbonyl iron powder is 3.5 mu m, and the density is 7.9g/cm3。
The magnetic Fe3O4Has an average particle size of 20 nm.
The carrier fluid is a polyolefin synthetic oil.
The gelatin is a coating agent, and can improve the agglomeration and sedimentation performance of magnetic particles.
The multi-walled carbon nano-tube is a cross-linking agent, and can improve the rheological property of the magnetic particles.
The stabilizer is sodium chloride.
The dispersant is oleic acid.
The dispersing agent is polyethylene glycol.
Example 1:
a preparation method of a double-dispersion magnetorheological fluid comprises the following steps:
Step 2, acidification of the multi-walled carbon nanotube: mixing nitric acid and sulfuric acid according to a molar ratio of 3:1 to prepare a strong acid mixed solution; adding the multi-walled carbon nano-tube into the mixed solution, heating to 55 ℃, and performing ultrasonic irradiation for 12h to obtain a strong acid acidified multi-walled carbon nano-tube solution.
Step 3, crosslinking of the multi-wall carbon nano-tubes: and (2) adding the magnetic particles obtained in the step (1) into the solution prepared in the step (2) for a crosslinking reaction, performing ultrasonic oscillation for 12 hours to crosslink the multi-wall carbon nano tubes on the surfaces of the magnetic particles, separating the coated magnetic particles under the action of a magnetic field, repeatedly washing with distilled water, and drying.
Step 4, synthesis of magnetorheological fluid: respectively adding the magnetic particles with the treated surfaces, graphite and polyethylene glycol into polyolefin synthetic oil, heating for 50min in a water bath environment at 60 ℃, starting a magnetic stirrer to stir, wherein the stirring speed is not too fast or too slow, and a tiny vortex is generated on the liquid level in a beaker until the uniform double-dispersion magnetorheological fluid is obtained.
The invention relates to a double-dispersion magnetorheological fluid and a preparation method thereof. At present, the main factors influencing the performance of the magnetorheological fluid are the sedimentation stability and the rheological performance of the magnetorheological fluid. The invention adds a small amount of nano-scale magnetic Fe into micron-scale carbonyl iron powder3O4Particles, and gelatin and multi-wall carbon nano-tubes are adopted to wrap carbonyl iron powder and Fe3O4As a dispersed phase, a double-dispersion magnetorheological fluid is prepared. The preparation process comprises the following steps: firstly, carbonyl iron powder, Fe3O4Adding the powder and the stabilizer into a gelatin aqueous solution according to a certain molar ratio, carrying out ultrasonic oscillation, carrying out magnetic separation, washing and drying to obtain the magnetic particles. And then placing the solution in an acidified multi-wall carbon nano tube solution, and carrying out ultrasonic oscillation again, separation, washing and drying. And finally, adding the surface-treated magnetic particles, the dispersing agent and the surfactant into the carrier liquid respectively for magnetic stirring to obtain the uniform double-dispersion magnetorheological fluid. The method comprises four steps of coating gelatin, acidifying multi-walled carbon nano-tubes, crosslinking the multi-walled carbon nano-tubes and synthesizing the magnetorheological fluid. The invention not only can obviously improve the sedimentation stability of the magnetorheological fluid, but also can enhance the magnetism and rheological property of the magnetorheological fluid, and can be widely applied to the industrial fields of aerospace, vehicles, machinery and the like.
Claims (7)
1. A preparation method of a double-dispersion magnetorheological fluid is characterized by comprising the following steps:
step one, wrapping gelatin: putting 2.5g of gelatin solid into 25ml of distilled water, and heating in a water bath environment until the gelatin is completely dissolved; 4g of carbonyl iron powder, 0.5g of magnetic Fe3O4Mixing with 0.2g sodium chloride solid, adding into gelatin water solution, and performing ultrasonic oscillation to coat carbonyl iron powder and Fe uniformly on gelatin layer3O4Separating the coated magnetic particles under the action of a magnetic field, washing the coated magnetic particles repeatedly with distilled water, and drying the magnetic particles;
step two, acidifying the multi-wall carbon nano tube: mixing nitric acid and sulfuric acid according to a molar ratio of 3:1 to prepare a strong acid mixed solution; adding the multi-walled carbon nanotube into the mixed solution, heating to 55-65 ℃, and performing ultrasonic irradiation for 12 hours to obtain a strong acid acidified multi-walled carbon nanotube solution;
step three, crosslinking of the multi-wall carbon nano-tubes: adding the magnetic particles obtained in the step (1) into the solution prepared in the step (2) for crosslinking reaction, performing ultrasonic oscillation to crosslink the multi-walled carbon nanotubes on the surfaces of the magnetic particles, separating the coated magnetic particles under the action of a magnetic field, repeatedly washing with distilled water, and drying;
step four, synthesizing magnetorheological fluid: respectively adding the magnetic particles, graphite and polyethylene glycol subjected to surface treatment into polyolefin synthetic oil, placing the polyolefin synthetic oil in a water bath environment for heating, starting a magnetic stirrer for stirring, wherein the stirring speed is not too high or too low, and a tiny vortex is generated on the liquid level in a beaker until uniform double-dispersion magnetorheological fluid is obtained;
the double-dispersion magnetorheological fluid comprises carbonyl iron powder and magnetic Fe3O4Carrier liquid, gelatin, multi-walled carbon nanotubes, a stabilizer, a dispersant and a surfactant; the mass fraction of the carbonyl iron powder is more than 98 percent; the magnetic Fe3O4Is more than 80 percent; the mass fraction of the carrier liquid is 20-30%; the multi-wall carbon nano tube accounts for 10 to 15 percent; the mass fraction of the stabilizer is 3-4%; the mass fraction of the dispersant is 1-3%; the mass fraction of the surfactant is 1-3%.
2. The preparation method of the double-dispersion magnetorheological fluid according to claim 1, which is characterized by comprising the following steps: the average grain diameter of the carbonyl iron powder is 3.5 mu m, and the density is 7.9g/cm3。
3. The preparation method of the double-dispersion magnetorheological fluid according to claim 1, which is characterized by comprising the following steps: the magnetic Fe3O4Has an average particle size of 20 nm.
4. The preparation method of the double-dispersion magnetorheological fluid according to claim 1, which is characterized by comprising the following steps: the carrier liquid is polyolefin synthetic oil; gelatin as coating agent, multi-wall carbon nano-tube as cross-linking agent, stabilizer as sodium chloride, dispersant as oleic acid, and surfactant as polyethylene glycol.
5. The preparation method of the double-dispersion magnetorheological fluid according to claim 1, which is characterized by comprising the following steps: in the first step, the water bath heating temperature is set to be 45-55 ℃, the time is set to be 30min, and the ultrasonic oscillation time is 5-7 h.
6. The preparation method of the double-dispersion magnetorheological fluid according to claim 1, which is characterized by comprising the following steps: in the third step, the ultrasonic oscillation time is 10-12 h.
7. The preparation method of the double-dispersion magnetorheological fluid according to claim 1, which is characterized by comprising the following steps: in the fourth step, the water bath heating temperature is set to be 50-60 ℃, and the time is set to be 50-60 min.
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| CN114518453B (en) * | 2022-01-26 | 2023-05-16 | 东北农业大学 | Multi-wall carbon nano tube compound and preparation method and application thereof |
| CN115302902B (en) * | 2022-07-06 | 2024-01-26 | 河南工业大学 | Flexible magnetic sensor and preparation method thereof |
| CN115746502B (en) * | 2022-11-09 | 2024-04-12 | 华中科技大学 | Quick curing and forming process for epoxy resin based on electromagnetic induction heating |
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