CN107459821A - A kind of silicon rubber magnetorheological elastomer composite material and preparation method thereof - Google Patents
A kind of silicon rubber magnetorheological elastomer composite material and preparation method thereof Download PDFInfo
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- CN107459821A CN107459821A CN201710928850.1A CN201710928850A CN107459821A CN 107459821 A CN107459821 A CN 107459821A CN 201710928850 A CN201710928850 A CN 201710928850A CN 107459821 A CN107459821 A CN 107459821A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The present invention relates to a kind of silicon rubber magnetorheological elastomer composite material and preparation method thereof, belong to field of material technology.Take carbonyl iron, Nd-Fe-B powder, isopropanol is fitted into ball milling in ball mill, dry, ferromagnetic particle must be pre-processed, take silane coupler neopelex, add in absolute ethyl alcohol, stirring, obtain modification liquid, pretreatment ferromagnetic particle is added into modification liquid, it is fitted into ball milling in ball mill after well mixed, filter residue is filtered to obtain after standing, filter residue is placed in drying box and dried, ferromagnetic particle must be modified, take modified ferromagnetic particle, dimethicone, silicon rubber, it is placed in after well mixed in vacuum drying chamber, the standing and defoaming in the case where vacuum is 10 ~ 30kPa, reinject in chilled glass die, it is placed in magnet charger, magnetize in 600 ~ 800mT uniform magnetic field, stand solidification at room temperature again, it is stripped to obtain silicon rubber magnetorheological elastomer composite material.
Description
Technical field
The present invention relates to a kind of silicon rubber magnetorheological elastomer composite material and preparation method thereof, belongs to material technology neck
Domain.
Background technology
In daily life, impact is ubiquitous, as car crass, aircraft landing, Canon launching, railway carriage touch
Hit, it is inestimable by being brought to the health of apparatus structure with human life if the transmission power of impact loading is not relaxed
Injury.Shown according to dynamics research, the reasonable application of buffer unit is one of effective way for relaxing shock loading, effectively
Reduction shock loading injured to caused by lives and properties.In Hyundai Motor design, mainly using V-type induction groove, built-in suction
Can the technology such as beam, reinforcing plate and energy-absorbing module to lift the security performance that automobile passively collides；And in the bumper of Hyundai Motor
In design, generally use filled polyurethane and resin realize passive buffering；Some high-grade cars using hydraulic bjuffer, air bag and
Pneumatic-control type buffer unit realizes passive buffering, security performance that lifting automobile passively collides.Aircraft landing gear, generally use
Rubber wheel relaxes the impact that airframe is faced when landing with hydraulic spring grease cup device, spring friction.Canon launching is usual
Using buffer units such as hydraulic spring type, metal-rubber, spring frictions, impact of the Canon launching to launcher, lifting are relaxed
The launcher life-span, and lift the hit rate of weapon.It is generally use pilot beam between the compartment of rail vehicle, coupler draft gear, anti-
The impact climbed between the absorption such as buffer, energy absorbing element compartment；Optimize the horizontal collapse structure of vehicle body simultaneously, lift track
The security performance of vehicle collision.Although above-mentioned passive buffer unit can play a part of to relax impact, above-mentioned is passive
The energy absorption characteristics of buffer unit are uncontrollable, it is impossible to the greatest extent to inhale according to impact velocity, quality, the parameter of type adjustment buffer unit more
Impact energy is received, protection mechanical structure preserves from.The controllable intellectual material of mechanical characteristic mainly has er material and magnetic current
Become material, its research and development brings new solution method to relax shock loading.Er material is by American scholar
Winslow 1947 find, found in subsequent research its exist shear yield stress is smaller, insulating requirements are high,
The fatal defects such as power consumption is big, impurity sensitivity, and then limit the engineer applied of er material.To mechanical characteristic controllable intelligent material
The research of material focuses primarily upon the research to magnetorheological materials and magnetorheological device, in view of the property of two kinds of materials is similar, thus
The part achievement in research of ER fluid, is equally applicable to magnetorheological materials.Then, magnetorheological materials family is also by initial magnetic current
Become liquid, occur the newcomers such as magneto-rheological grease, magnetic rheology elastic body, magnetorheological foam, magnetorheological glue, magnetorheological plastic body successively.
Magnetorheological materials are a kind of the multidirectional mixture that corresponding modifying agent forms to be equipped with by carrier and magnetizable particles.Magnetic-particle is
Crystallite dimension is in 0.01~50um scopes, if particle size is too small, makes the magnetorheological poor-performing of the magnetorheological materials of preparation；If
Particle size is excessive, then makes the less stable of the magnetic material of preparation and be not easy to be dispersed in carrier.Magnetic-particle one
As select have heat endurance it is good（Curie temperature is high）, ferromagnetic of the advantages that oxidation resistance is strong, magnetic conductivity is high, coercivity is small
Grain（Such as ferrocobalt, iron-nickel alloy, carbonyl iron dust）.Carrier mainly from good stability, it is nontoxic, to environment without dirt
Dye, not magnetic conduction the features such as material, preferably have organic material and inorganic material dual property concurrently, make the magnetorheological materials of preparation have
Good high-temperature behavior and cryogenic property.Effect in magnetic field, magnetic-particle along magnetic induction line direction arrangement form magnetic linkage, so as to
Change the mechanical property of material.Additive is used for the compatibility of lifting carrier and magnetic-particle so that the magnetorheological materials of preparation
With good stability and more preferable mechanical property.
The content of the invention
The technical problems to be solved by the invention：For existing magnetorheological materials in damping of shocks field Shortcomings, sink
The problem of poor stability, Acclimation temperature narrow range, adjustable extent are narrow, and shear yielding power is low is dropped, there is provided a kind of silicon rubber magnetic current
Become elastic composite and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of silicon rubber magnetorheological elastomer composite material, including following weight parts raw material are made：
60 ~ 80 parts of modified ferromagnetic particles, 10 ~ 15 parts of dimethicones, 15 ~ 20 parts of silicon rubber.
The modified ferromagnetic particle is carbonyl iron, is made after Nd-Fe-B powder pretreatment through modification liquid modification.
The modification liquid is by 1.2 ~ 1.6 parts by weight silane resin acceptor kh-550s, 2.4 ~ 3.2 parts by weight detergent alkylate sulphurs
Sour sodium, 120~160 parts by weight absolute ethyl alcohols composition.
The preprocessing process is that carbonyl iron, Nd-Fe-B powder, isopropanol are fitted into ball milling in ball mill, then in vacuum is 10
~ 30kPa, dry to constant weight at 200 ~ 240 DEG C.
The carbonyl iron, Nd-Fe-B powder, the parts by weight of isopropanol are 50 ~ 60 parts of carbonyl irons, 10 ~ 20 parts of Nd-Fe-B powders, 2.0
~ 2.4 parts of isopropanols.
The modification is by modification liquid and pretreatment ferromagnetic particle in mass ratio 2：After 1 is well mixed, with 300 ~
400r/min 5 ~ 6h of ball milling, stand filtration drying after 3 ~ 5h.
The silicon rubber is condensed room temperature vulcanized silicone rubber.
The preparation method of described a kind of silicon rubber magnetorheological elastomer composite material, it is characterised in that concretely comprise the following steps：
S1. take carbonyl iron, Nd-Fe-B powder, isopropanol ball milling mixing uniform, then be dried in vacuo, obtain pretreatment ferromagnetic particle；
S2. modification liquid is prepared；
S3. ball milling is stood after modification liquid is well mixed with pretreatment ferromagnetic particle, and filtration drying must be modified ferromagnetic particle；
S4. ferromagnetic particle, dimethicone, silicon rubber will be modified, 20 ~ 30min of vacuum defoamation, reinjects tempering after being well mixed
In glass mold, it is placed in magnet charger, magnetizes 30 ~ 40min in 600 ~ 800mT uniform magnetic field, then stand at room temperature
Solidify 2 ~ 3h, be stripped to obtain silicon rubber magnetorheological elastomer composite material.
Compared with other method, advantageous effects are the present invention：
（1）The present invention is increased the mobility of silicon rubber by dimethicone, plays lubrication, just using silicon rubber as matrix
Disperse in movement of the modified ferromagnetic particle in matrix, while increase the suppleness of silicon rubber, reduce null field modulus, and it is magnetorheological
Material is in semi-solid state, has mushy stage material dual performance so that the controlled range of magnetic rheology elastic body is wider；
（2）The present invention occurs condensation reaction by silane coupler and the hydroxyl on ferromagnetic particle surface and forms covalent bond, and silane is each
The silanol of the molecule film that mutual association oligomerisation forms network structure again is covered in particle surface, makes ferromagnetic particle surface organic,
The associativity of modified ferromagnetic particle and silicon rubber is improved, improves sedimentation stability；
（3）Silicon rubber magnetorheological elastomer composite material prepared by the present invention have sedimentation stability is good, Acclimation temperature scope is wide,
Adjustable extent is wide, shear yield stress more than 100kPa the features such as, it is slow in impact can effectively to make up existing magnetorheological materials
Rush the deficiency of field application.
Embodiment
50 ~ 60g carbonyl irons are taken, 10 ~ 20g Nd-Fe-B powders, 2.0 ~ 2.4g isopropanols are fitted into ball mill, with 180 ~ 200r/
Min 50 ~ 60min of ball milling, then be transferred in vacuum drying chamber, it is 10 ~ 30kPa in vacuum, is dried at 200 ~ 240 DEG C to constant weight,
Ferromagnetic particle must be pre-processed, 1.2~1.6g silane resin acceptor kh-550s is taken, 2.4 ~ 3.2g neopelexes, adds 120
In~160g absolute ethyl alcohols, 20 ~ 30min is stirred with 300~400r/min, modification liquid is obtained, is added into 120 ~ 160g modification liquids
60 ~ 80g pre-processes ferromagnetic particle, is fitted into after well mixed in ball mill, with 300 ~ 400r/min, 5 ~ 6h of ball milling, after 3 ~ 5h of standing
Filter residue is filtered to obtain, filter residue is placed in drying box, 3 ~ 5h is dried at 70 ~ 80 DEG C, obtains modified ferromagnetic particle, takes 60 ~ 80g to be modified
Ferromagnetic particle, 10 ~ 15g dimethicones, 15 ~ 20g silicon rubber, it is placed in after well mixed in vacuum drying chamber, is in vacuum
20 ~ 30min of standing and defoaming under 10 ~ 30kPa, is reinjected in chilled glass die, is placed in magnet charger, 600 ~ 800mT's
Magnetize 30 ~ 40min in uniform magnetic field, then stand 2 ~ 3h of solidification at room temperature, be stripped to obtain silicon rubber magnetic rheology elastic body composite wood
Material.
Example 1
50g carbonyl irons, 10g Nd-Fe-B powders are taken, 2.0g isopropanols are fitted into ball mill, with 180r/min ball milling 50min, then are transferred to
In vacuum drying chamber, it is 10kPa in vacuum, is dried at 200 DEG C to constant weight, obtain pretreatment ferromagnetic particle, take 1.2g silane even
Join agent KH-550,2.4g neopelex, add in 120g absolute ethyl alcohols, 20min is stirred with 300r/min, obtains modification
Liquid, 60g pretreatment ferromagnetic particles are added into 120g modification liquids, are fitted into after well mixed in ball mill, with 300r/min ball millings
5h, filter residue is filtered to obtain after standing 3h, filter residue is placed in drying box, 3h is dried at 70 DEG C, modified ferromagnetic particle is obtained, takes 60g
Modified ferromagnetic particle, 10g dimethicones, 15g silicon rubber, is placed in vacuum drying chamber after well mixed, is in vacuum
Standing and defoaming 20min under 10kPa, is reinjected in chilled glass die, is placed in magnet charger, in 600 mT uniform magnetic field
Magnetize 30min, then stand solidification 2h at room temperature, be stripped to obtain silicon rubber magnetorheological elastomer composite material.
Example 2
55g carbonyl irons, 15g Nd-Fe-B powders are taken, 2.2g isopropanols are fitted into ball mill, with 190r/min ball milling 55min, then are transferred to
In vacuum drying chamber, it is 20kPa in vacuum, is dried at 220 DEG C to constant weight, obtain pretreatment ferromagnetic particle, take 1.4g silane even
Join agent KH-550,2.8g neopelex, add in 140g absolute ethyl alcohols, 25min is stirred with 350r/min, obtains modification
Liquid, 70g pretreatment ferromagnetic particles are added into 140g modification liquids, are fitted into after well mixed in ball mill, 350r/min ball milling 5h,
Filter residue is filtered to obtain after standing 4h, filter residue is placed in drying box, 4h is dried at 75 DEG C, modified ferromagnetic particle is obtained, takes 70g to be modified
Ferromagnetic particle, 13g dimethicones, 17g silicon rubber, it is placed in after well mixed in vacuum drying chamber, in the case where vacuum is 20kPa
Standing and defoaming 250min, is reinjected in chilled glass die, is placed in magnet charger, is magnetized in 700mT uniform magnetic field
35min, then solidification 2h is stood at room temperature, it is stripped to obtain silicon rubber magnetorheological elastomer composite material.
Example 3
60g carbonyl irons, 20g Nd-Fe-B powders are taken, 2.4g isopropanols are fitted into ball mill, with 200r/min ball milling 60min, then are transferred to
In vacuum drying chamber, it is 30kPa in vacuum, is dried at 240 DEG C to constant weight, obtain pretreatment ferromagnetic particle, take 1.6g silane even
Join agent KH-550,3.2g neopelex, add in 160g absolute ethyl alcohols, 30min is stirred with 400r/min, obtains modification
Liquid, 80g pretreatment ferromagnetic particles are added into 160g modification liquids, are fitted into after well mixed in ball mill, with 400r/min ball millings
6h, filter residue is filtered to obtain after standing 5h, filter residue is placed in drying box, 5h is dried at 80 DEG C, modified ferromagnetic particle is obtained, takes 80g
Modified ferromagnetic particle, 15g dimethicones, 20g silicon rubber, is placed in vacuum drying chamber after well mixed, is in vacuum
Standing and defoaming 30min under 30kPa, is reinjected in chilled glass die, is placed in magnet charger, in 800mT uniform magnetic field
Magnetize 40min, then stand solidification 3h at room temperature, be stripped to obtain silicon rubber magnetorheological elastomer composite material.
The magnetorheological materials that a kind of silicon rubber magnetorheological elastomer composite material being prepared into and Anhui company are produced
Detected, specific detection is as follows：
（1）The coefficient of rigidity is tested
Magnetorheological viscoelastic material is as a kind of viscous-elastic material in sinusoidal strain γ=γ0Under sin ω t effects, its stress
Relation between strain can be used to lower relation and represent：T=G* γ G* are complex shear modulus, are represented as follows：G*= G1+G2
Wherein, G* is modulus of elasticity, and it is directly proportional in the average value of the stored energy of certain deformation to the material of unit volume, shows
Material resists the ability of additional deformation；Its value is bigger, it is meant that the ability that material resists additional deformation is stronger.G* is loss mould
Amount, refers to material when deforming upon, due to viscous deformation（It is irreversible）And the energy size being lost, reflection tack of materials are big
It is small.MCR-301 is a kind of rheological behavior test system, to conditions such as frequency of oscillation, strain, test gaps, is automatically performed test
And calculate dynamic mechanics parameter according to the data of collection.
（2）Rheologic behavio(u)r is tested
Rheologic behavio(u)r is one of most important index of performance for weighing magnetorheological materials, for the magnetorheological viscoplasticity of evaluation preparation
The flowing energy-dissipating property of material, its rheologic behavio(u)r need to be tested, preparation technology is optimized and to damp by test data
Device design provides crucial parameter.
（3）Shear yielding power is tested
Influence that the factor of the shear stress of magnetorheological viscoelastic material is a lot, can when material and the timing of particle diameter one of carbonyl iron dust
The concentration of magnetized particles plays main function to the shear stress of magnetorheological viscoelastic material.Test condition is：Exciting current model
Enclose for（0~3A）, shearing rate 200s-1, testing radius 10mm, test gap 1mm, number of test points 31.
（4）Standing sedimentation is observed
, need to be to magnetic to prevent carbonyl iron dust from producing sedimentation under gravity because the density of carbonyl iron dust is much larger than matrix
Rheo-material is correspondingly processed, to prevent material magnetic rheology effect from failing.For magnetic flow liquid, magnetic under gravity
The sedimentation of particle is unavoidable, although passing through the surface treatment to particle so that particle can be in the condition of extraneous vibration
Under, it is dispersed in carrier fluid, but have little time dispersed for shock loading, magnetic-particle.Therefore, it is necessary to test
The standing sedimentation stability of magnetorheological viscoelastic material, it is that it is used for the key index of shock loading.Specific test result such as table
1。
The silicon rubber magnetorheological elastomer composite material performance characterization of table 1
As shown in Table 1, the silicon rubber magnetorheological elastomer composite material for preparing of the present invention has that sedimentation stability is good, Acclimation temperature
Scope is wide, adjustable extent is wide, shear yield stress more than 100kPa the features such as, can effectively make up existing magnetorheological materials and exist
The deficiency of damping of shocks field application.
Claims (8)
1. a kind of silicon rubber magnetorheological elastomer composite material, it is characterised in that be made including following weight parts raw material：
60 ~ 80 parts of modified ferromagnetic particles, 10 ~ 15 parts of dimethicones, 15 ~ 20 parts of silicon rubber.
2. a kind of silicon rubber magnetorheological elastomer composite material as claimed in claim 1, it is characterised in that described to change
Property ferromagnetic particle be carbonyl iron, Nd-Fe-B powder pretreatment after be made through modification liquid modification.
3. a kind of silicon rubber magnetorheological elastomer composite material as claimed in claim 2, it is characterised in that described to change
Property liquid be 2.4 ~ 3.2 parts by weight neopelexes by 1.2 ~ 1.6 parts by weight silane resin acceptor kh-550s, 120~
160 parts by weight absolute ethyl alcohols form.
4. a kind of silicon rubber magnetorheological elastomer composite material as claimed in claim 2, it is characterised in that described pre-
Processing procedure is that carbonyl iron, Nd-Fe-B powder, isopropanol are fitted into ball milling in ball mill, then in vacuum is 10 ~ 30kPa, 200
Dried at ~ 240 DEG C to constant weight.
A kind of 5. silicon rubber magnetorheological elastomer composite material as claimed in claim 4, it is characterised in that the carbonyl iron,
Nd-Fe-B powder, the parts by weight of isopropanol are 50 ~ 60 parts of carbonyl irons, 10 ~ 20 parts of Nd-Fe-B powders, 2.0 ~ 2.4 parts of isopropanols.
A kind of 6. silicon rubber magnetorheological elastomer composite material as claimed in claim 2, it is characterised in that the modification
For by modification liquid with pretreatment ferromagnetic particle in mass ratio 2：After 1 is well mixed, with 300 ~ 400r/min, 5 ~ 6h of ball milling, 3 are stood ~
Filtration drying after 5h.
7. a kind of silicon rubber magnetorheological elastomer composite material as claimed in claim 1, it is characterised in that the silicon rubber is
Condensed room temperature vulcanized silicone rubber.
8. a kind of preparation method of silicon rubber magnetorheological elastomer composite material as described in claim 1 ~ 7 any one, its
It is characterised by, concretely comprises the following steps：
S1. take carbonyl iron, Nd-Fe-B powder, isopropanol ball milling mixing uniform, then be dried in vacuo, obtain pretreatment ferromagnetic particle；
S2. modification liquid is prepared；
S3. ball milling is stood after modification liquid is well mixed with pretreatment ferromagnetic particle, and filtration drying must be modified ferromagnetic particle；
S4. ferromagnetic particle, dimethicone, silicon rubber will be modified, 20 ~ 30min of vacuum defoamation, reinjects tempering after being well mixed
In glass mold, it is placed in magnet charger, magnetizes 30 ~ 40min in 600 ~ 800mT uniform magnetic field, then stand at room temperature
Solidify 2 ~ 3h, be stripped to obtain silicon rubber magnetorheological elastomer composite material.
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Cited By (7)
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| CN108727710A (en) * | 2018-06-05 | 2018-11-02 | 重庆大学 | Preparation method with high heat-resisting and tensile properties magnetic rheology elastic body |
| CN109295844A (en) * | 2018-10-30 | 2019-02-01 | 扬州大学 | A kind of magnetorheological high damping elastomer single support of laminated type |
| CN110000619A (en) * | 2019-03-12 | 2019-07-12 | 湘潭大学 | Micro- texture flexible abrasive wheel of magnetorheological glue and preparation method thereof and grinding attachment |
| CN110246643A (en) * | 2019-07-11 | 2019-09-17 | 赖松平 | A kind of rail traffic vehicles motor high-performance bonded NdFeB Permanent magnet composite material |
| CN113733545A (en) * | 2021-08-31 | 2021-12-03 | 兰州大学 | Preparation method of magnetic-sensitive intelligent superstructure |
| CN113770816A (en) * | 2021-09-09 | 2021-12-10 | 广东工业大学 | Magnetorheological elastomer and preparation method and application thereof |
| CN115093705A (en) * | 2022-08-08 | 2022-09-23 | 河南工业大学 | Neodymium-iron-boron-based organic composite material, frog-imitating soft robot and preparation method thereof |
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| CN110246643A (en) * | 2019-07-11 | 2019-09-17 | 赖松平 | A kind of rail traffic vehicles motor high-performance bonded NdFeB Permanent magnet composite material |
| CN113733545A (en) * | 2021-08-31 | 2021-12-03 | 兰州大学 | Preparation method of magnetic-sensitive intelligent superstructure |
| CN113770816A (en) * | 2021-09-09 | 2021-12-10 | 广东工业大学 | Magnetorheological elastomer and preparation method and application thereof |
| CN115093705A (en) * | 2022-08-08 | 2022-09-23 | 河南工业大学 | Neodymium-iron-boron-based organic composite material, frog-imitating soft robot and preparation method thereof |
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Application publication date: 20171212 |