CN114334414A - Preparation process of anti-settling magnetorheological fluid of soft magnetic composite particles - Google Patents
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Abstract
The invention discloses a preparation process of anti-settling magnetorheological fluid of soft magnetic composite particles. The anti-settling magnetorheological fluid is prepared by placing the soft magnetic composite particles and the surface additive in absolute ethyl alcohol by adopting a base fluid displacement method, carrying out modification coating treatment on the soft magnetic composite particles by constant-temperature high-speed mechanical stirring, high-speed ball milling, drying and dispersing, and then adding materials such as base carrier fluid, thixotropic agent, lubricant and the like for secondary high-speed stirring. The soft magnetic composite particles used in the invention are carbonyl iron powder and Fe-Co-Ni porous metal cellular ternary alloy nano powder with specified particle size, the base carrier liquid is dimethyl silicone oil, and 2-5% of various surfactants, 1-2% of thixotropic agents and 1-2% of lubricating agents are used. And measuring performance parameters such as sedimentation stability, apparent viscosity, shear yield stress and the like by using a rotational viscometer, a rheometer and a standing method. The result shows that the prepared anti-sedimentation magnetorheological fluid of the soft magnetic composite particles can effectively improve the sedimentation stability.
Description
Technical Field
The invention relates to the technical field of intelligent material preparation, in particular to a preparation process of anti-settling magnetorheological fluid of soft magnetic composite particles.
Background
The magnetorheological fluid is a novel intelligent material, belongs to a typical coarse dispersion system, mainly comprises three parts, namely soft magnetic particles, base carrier fluid and additives, and the self characteristics of each part have decisive influence on the performance of the magnetorheological fluid. Wherein, the soft magnetic particles are the determining factor of the magnetic property of the magnetorheological fluid; the base carrier liquid is a determining factor of the flow characteristic and the sedimentation stability of the magnetorheological fluid when the dispersed phase of the soft magnetic particles is used as the base carrier liquid; the additive has the effect of improving various comprehensive properties of the magnetorheological fluid. The magnetorheological fluid can generate a unique magnetorheological effect under the action of an external magnetic field, and is specifically represented in that under a macroscopic state, the magnetorheological fluid is influenced by the external magnetic field, and can be converted from a Newton fluid capable of flowing freely into a Bingham fluid similar to a solid; under the microscopic state, the soft magnetic particles in the base carrier liquid are gathered into a chain, column or net-shaped stable structure in the direction of magnetic force lines in the base carrier liquid, and the change is rapid and reversible. The magnetorheological fluid has unique rheological property, simple and convenient speed regulation, high response speed and good constant torque property, and is widely applied to the fields of dampers, shock absorbers, transmission devices (clutches, brakes and the like), polishing devices, composite members and the like.
At present, most of magnetorheological fluid is used for dampers and shock absorbers, and the research on the magnetorheological fluid for transmission is relatively less. Meanwhile, most scholars have conducted many researches on the base carrier fluid and additives in the three components of the magnetorheological fluid, such as the chinese patent published in 2021, 3 months and 26 days: in the preparation method (publication number: CN112552987A) of the hyperstable silicon oil-based magnetorheological fluid, the research is carried out on the types and the compounding method of the additives, the traditional complicated steps are optimized, and the complex reaction conditions are met, so that the magnetorheological fluid product with more excellent performance is obtained; chinese patent published on 5/14/2021: research on thixotropic agents and lubricants is carried out in high-performance magnetorheological fluids using graphene-carbon nanotube compound particles as anti-settling agents and preparation methods (publication number: CN109337742B) of the high-performance magnetorheological fluids, and the fact that the sedimentation stability and the zero-field viscosity of the magnetorheological fluids can be effectively improved by using graphene or carbon nanotubes as the anti-settling agents is found. However, domestic patents have less research on soft magnetic particles, and the main reason for the sedimentation of the magnetorheological fluid is the large density difference between the soft magnetic particles and the base carrier fluid. Therefore, research is carried out on the soft magnetic composite particles, and the sedimentation stability of the magnetorheological fluid can be effectively improved on the basis of balancing various performances of the magnetorheological fluid.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a preparation process of anti-settling magnetorheological fluid of soft magnetic composite particles, wherein the proportion of the soft magnetic particles is adjusted, and nano-scale Fe-Co-Ni porous metal cellular ternary alloy powder is added to balance the density difference between the soft magnetic particles and base carrier fluid. Meanwhile, the sedimentation of micron-sized carbonyl iron powder particles is inhibited by utilizing the electrostatic repulsion and steric hindrance between the nano particles; the micron-sized particles and the nanometer-sized particles in the soft magnetic particles are magnetic conductive metal particles, the micron-sized particles are mainly used, and the characteristics of the prepared magnetorheological fluid such as shear yield stress, response time and the like cannot be greatly influenced.
The invention adopts the following technical scheme:
the anti-settling magnetorheological fluid is prepared by placing the soft magnetic composite particles and the surface additive in absolute ethyl alcohol by a base fluid replacement method, performing constant-temperature high-speed mechanical stirring, high-speed ball milling, drying and dispersing, adding base carrier fluid, thixotropic agent, lubricant and other materials after the modified coating treatment of the soft magnetic composite particles, and performing secondary high-speed stirring.
Wherein the soft magnetic composite particles, the base carrier liquid and the additive are as follows by mass percent: 65-70% of soft magnetic composite particles, 20-30% of base carrier liquid and 5-10% of additive.
Furthermore, the soft magnetic composite particles are formed by compounding carbonyl iron powder with a regular spherical structure, uniform particle size distribution and an average particle size of 2 mu m and porous honeycomb Fe-Co-Ni ternary alloy nano metal powder.
Further, the soft magnetic composite particles comprise the following components in percentage by mass: 85-95% of carbonyl iron powder and 5-15% of Fe-Co-Ni porous metal honeycomb structure nano powder.
Further, the base carrier fluid is dimethyl silicone oil with excellent high-temperature stability and viscosity-temperature characteristics, and the kinematic viscosity is 100 Cst.
Further, the additive comprises the following components in percentage by mass: 4-6% of surfactant, 1-2% of thixotropic agent and 1-2% of lubricant
Further, the surfactant is at least one of sodium dodecyl benzene sulfonate, composite MES, sodium lauryl phosphate and ethylene glycol monostearate.
Further, the thixotropic agent is at least one of fumed silica, white carbon black and organic bentonite.
Further, the lubricant is at least one of molybdenum dioxide, boron nitride or diamond.
Further, the preparation process adopts a base liquid displacement method, and comprises the following specific steps:
1) mixing a proper amount of soft magnetic composite particles with a surfactant, adding the mixture into absolute ethyl alcohol, stirring for 6 hours at the rotating speed of 400r/min and the oil bath temperature of 40 ℃, and drying and carrying out high-temperature treatment in a vacuum drying oven at the temperature of 220 ℃;
2) putting the mixture treated in the step 1) into a ball mill for grinding for 1h, and dispersing for 15 minutes by using an ultrasonic dispersion machine to prevent agglomeration;
3) and adding the carrier liquid, the thixotropic agent and the lubricant into the carbonyl iron powder treated in the step 2), and stirring for 1 hour by using a ball mill.
Compared with the prior art, the invention has the beneficial effects that:
(1) the composite soft magnetic particles are prepared by adding porous metal cellular Fe-Co-Ni ternary alloy nano powder into common micron-sized carbonyl iron powder particles to balance the density difference between the soft magnetic particles and a base carrier fluid. Meanwhile, the sedimentation of micron-sized carbonyl iron powder particles is inhibited by utilizing the electrostatic repulsion and steric hindrance between the nano particles;
(2) the micron-sized particles and the nanometer-sized particles in the soft magnetic composite particles adopt high-magnetic-permeability metal particles, so that the settling stability of the magnetorheological fluid is improved, and the performances such as shear yield stress, rheological response time and the like are balanced;
(3) the Fe-Co-Ni ternary alloy nano powder is in a porous metal honeycomb structure, so that the coating effect of additives such as a surfactant, a coupling agent and the like on the surface of soft magnetic particles can be optimized, and various properties of the magnetorheological fluid can be optimized.
Drawings
FIG. 1 is a process flow diagram of a process for preparing an anti-settling magnetorheological fluid containing soft magnetic composite particles according to the present invention;
FIG. 2 is a process flow introduction of the base liquid displacement method.
Detailed Description
The features and principles of the present invention will be described in detail below with reference to the accompanying drawings and the detailed description, which are given by way of illustration only and are not intended to limit the scope of the invention.
The invention provides a preparation process of anti-settling magnetorheological fluid of soft magnetic composite particles, which comprises the following steps:
the anti-settling magnetorheological fluid is prepared by placing the soft magnetic composite particles and the surface additive in absolute ethyl alcohol by a base fluid replacement method, performing constant-temperature high-speed mechanical stirring, high-speed ball milling, drying and dispersing, adding base carrier fluid, thixotropic agent, lubricant and other materials after the modified coating treatment of the soft magnetic composite particles, and performing secondary high-speed stirring.
Wherein the soft magnetic composite particles, the base carrier liquid and the additive are as follows by mass percent: 65-70% of soft magnetic composite particles, 20-30% of base carrier liquid and 5-10% of additive.
Furthermore, the soft magnetic composite particles are formed by compounding carbonyl iron powder with a regular spherical structure, uniform particle size distribution and an average particle size of 2 mu m and Fe-Co-Ni porous metal honeycomb ternary alloy nano powder.
Further, the soft magnetic composite particles comprise the following components in percentage by mass: 85-95% of carbonyl iron powder and 5-15% of Fe-Co-Ni porous metal honeycomb structure nano powder.
Further, the base carrier fluid is dimethyl silicone oil with excellent high-temperature stability and viscosity-temperature characteristics, and the kinematic viscosity is 100 Cst.
Further, the additive comprises the following components in percentage by mass: 4-6% of surfactant, 1-2% of thixotropic agent and 1-2% of lubricant
Further, the surfactant is at least one of sodium dodecyl benzene sulfonate, composite MES, sodium lauryl phosphate and ethylene glycol monostearate.
Further, the thixotropic agent is at least one of fumed silica, white carbon black and organic bentonite.
Further, the lubricant is at least one of molybdenum dioxide, boron nitride or diamond.
Embodiment 1, a method for preparing a process for preparing a soft magnetic composite particle anti-settling magnetorheological fluid, comprising the following steps:
59.5g of carbonyl iron powder, 10.5g of nano Fe-Co-Ni powder, 2g of sodium lauryl phosphate, sodium dodecyl benzene sulfonate and composite MES mixed solution, 1g of molybdenum dioxide, 25g of silicone oil and 2g of silicon dioxide are weighed. Putting carbonyl iron powder and nano Fe-Co-Ni powder into a vacuum drying oven at the temperature of 220 ℃, keeping for 1 hour, taking out, removing the physical adsorption water on the surface of the carbonyl iron powder and carrying out high-temperature treatment on various materials.
A base liquid displacement method is adopted, sodium lauryl phosphate, sodium dodecyl benzene sulfonate, composite MES mixed solution and soft magnetic composite particles are added into a large amount of absolute ethyl alcohol, the mixture is placed into an ultrasonic disperser for dispersion, and the treated solution is maintained in an oil bath kettle for preparation at the constant temperature of 40 ℃, the rotating speed of a stirrer of 400r/min and the time of 6 hours.
Further, the mixture after stirring and dispersing was dried in a vacuum oven at a vacuum degree of 0.2MPa and a temperature of 80 ℃ for 1 hour. And redundant bubbles and absolute ethyl alcohol in the coated carbonyl iron powder can be volatilized through drying in a vacuum drying oven. Then, the carbonyl iron powder particles treated with the surfactant are subjected to high-speed ball milling by a ball mill, and at the same time, the dried material is dispersed by an ultrasonic disperser to prevent agglomeration.
Further, 25g of silicone oil, 2g of silicon dioxide and 1g of molybdenum dioxide were added to the treated carbonyl iron powder, and the mixture was stirred twice. The time of the secondary stirring process is 1 hour, the temperature is kept constant at 40 ℃ by adopting an oil bath kettle, and the rotating speed is 400 r/min. Then putting the mixture into a ball mill for ball milling treatment.
The magnetorheological fluid prepared by taking the prepared mixed solution of sodium lauryl phosphate, sodium dodecyl benzene sulfonate and composite MES as a surface additive, silicon dioxide as a thixotropic agent and molybdenum disulfide as a lubricant is tested by using an SNB-1T rotational viscometer, when the temperature is 25.9 ℃, the zero field viscosity is 0.983Pa.s, the shear yield stress measured by using an MCR-301 rheometer can reach 35.6kPa, a standing method is adopted, the sedimentation rate is 0.81 percent after one week, and the performance is excellent.
Comparative example 1
70g of carbonyl iron powder, 2g of sodium lauryl phosphate, sodium dodecyl benzene sulfonate and composite MES mixed solution, 1g of molybdenum dioxide, 25g of silicone oil and 2g of silicon dioxide are weighed. The carbonyl iron powder is placed in a vacuum drying oven at the temperature of 220 ℃, kept for 1 hour and then taken out, the physical adsorption water on the surface of the carbonyl iron powder is removed, and the high-temperature treatment is firstly carried out on various materials.
The other steps are carried out according to the example 1, the prepared comparison liquid has the zero field viscosity of 1.23Pa.s, the shear yield stress of 35.9kPa and the sedimentation rate of 4.61 percent after one week when the temperature is 25.9 ℃ measured by using an SNB-1T rotational viscometer, an MCR-301 rheometer and a standing method.
By combining the embodiment 1 and the comparative example 1, the magnetorheological fluid prepared by the preparation process of the anti-settling magnetorheological fluid containing the soft magnetic composite particles according to the type and the proportion of the composite soft magnetic particles has more excellent settling stability and lower zero-field viscosity, the shear yield stress is not obviously reduced on the basis of obviously improving the anti-settling effect of the magnetorheological fluid, the preparation process is simple, and the cost performance is higher.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the present invention by those skilled in the art without departing from the spirit of the present invention are intended to be covered by the protection scope defined by the claims of the present invention.
Claims (9)
1. A preparation process of anti-settling magnetorheological fluid of soft magnetic composite particles is characterized by comprising the following steps: placing the soft magnetic composite particles and the surface additive into absolute ethyl alcohol by adopting a base liquid displacement method, and performing constant-temperature high-speed mechanical stirring, high-speed ball milling, drying and dispersing to realize the modified coating treatment of the soft magnetic composite particles, and then adding materials such as base carrier liquid, thixotropic agent, lubricant and the like to perform secondary high-speed stirring to prepare the anti-settling magnetorheological fluid; wherein the soft magnetic composite particles, the base carrier liquid and the additive are as follows by mass percent: 65-70% of soft magnetic composite particles, 20-30% of base carrier liquid and 5-10% of additive.
2. The process for preparing a soft magnetic composite particle anti-settling magnetorheological fluid according to claim 1, wherein the process comprises the following steps: the soft magnetic composite particles are formed by compounding carbonyl iron powder with a regular spherical structure, uniform particle size distribution and an average particle size of 2 mu m and porous cellular Fe-Co-Ni ternary alloy nano metal powder.
3. The process for preparing a soft magnetic composite particle anti-settling magnetorheological fluid according to claim 2, wherein the process comprises the following steps: the soft magnetic composite particles comprise the following components in percentage by mass: 85-95% of carbonyl iron powder and 5-15% of Fe-Co-Ni porous metal honeycomb structure nano powder.
4. The process for preparing a soft magnetic composite particle anti-settling magnetorheological fluid according to claim 1, wherein the process comprises the following steps: the base carrier liquid adopts dimethyl silicone oil with excellent high-temperature stability and viscosity-temperature characteristics, and the kinematic viscosity is 100 Cst.
5. The process for preparing a soft magnetic composite particle anti-settling magnetorheological fluid according to claim 1, wherein the process comprises the following steps: the additive comprises the following components in percentage by mass: 4-6% of surfactant, 1-2% of thixotropic agent and 1-2% of lubricant.
6. The process for preparing a soft magnetic composite particle anti-settling magnetorheological fluid according to claim 1, wherein the process comprises the following steps: the surfactant is at least one of sodium dodecyl benzene sulfonate, composite MES, sodium lauryl phosphate and ethylene glycol monostearate.
7. The process for preparing a soft magnetic composite particle anti-settling magnetorheological fluid according to claim 1, wherein the process comprises the following steps: the thixotropic agent is at least one of fumed silica, white carbon black and organic bentonite.
8. The process for preparing a soft magnetic composite particle anti-settling magnetorheological fluid according to claim 1, wherein the process comprises the following steps: the lubricant is at least one of molybdenum dioxide, boron nitride or diamond.
9. The process for preparing a soft magnetic composite particle anti-settling magnetorheological fluid according to claim 1, wherein the process comprises the following steps: the magnetorheological fluid is prepared by a base fluid displacement method, and the method comprises the following specific steps:
1) mixing a proper amount of soft magnetic composite particles with a surfactant, adding the mixture into absolute ethyl alcohol, stirring for 6 hours at the rotating speed of 400r/min and the oil bath temperature of 40 ℃, and drying and carrying out high-temperature treatment in a vacuum drying oven at the temperature of 220 ℃;
2) grinding the mixture treated in the step 1) in a ball mill, and dispersing for 15 minutes by using an ultrasonic dispersion machine to prevent agglomeration;
3) and adding the carrier liquid, the thixotropic agent and the lubricant into the carbonyl iron powder treated in the step 2), and stirring for 1 hour by using a ball mill.
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| CN115295269A (en) * | 2022-08-14 | 2022-11-04 | 重庆大学 | Radiation-resistant magnetorheological fluid with high shear yield stress under low magnetic field |
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