CN105885198A - Preparing method of Fe3O4 nanometer chain composite film based on MEMS orientation - Google Patents
Preparing method of Fe3O4 nanometer chain composite film based on MEMS orientation Download PDFInfo
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Abstract
The invention discloses a preparing method of a Fe3O4 nanometer chain composite film based on MEMS orientation. The preparing method comprises the steps that a solution is synthesized into one-dimension permanent magnet Fe3O4 nanometer chains and synthesized into monodispersion Fe3O4 nanometer microspheres through a heating method; by means of an applied magnetic field, the monodispersion Fe3O4 nanometer microspheres are arranged according to the magnetic field direction to be subjected to a polymerization reaction, and under induction of a magnetic field, the Fe3O4 nanometer microspheres are assembled into a one-dimensional Fe3O4 nanometer chain; the Fe3O4 nanometer chain is added into an SBS/LLDPE blend solution, and dispersed on the ice bath condition; the composite film is initially formed, wherein a method for film forming through a rotary coating method is adopted for preparing the solution into the shape of the film initially, after a spin coater is utilized for absorbing pieces, the solution is added to a bottom plate, centrifugal force is utilized for dividing the solution uniformly, the spin coater is controlled to control the thickness of the solution, and the composite film is prepared. The composite film is fast in response, large in deformation amount and controllable in deformation, and has great research value and engineering significance.
Description
Technical field
The invention belongs to laminated film technical field, particularly relate to a kind of based on MEMS orientation Fe3O4Nanometer
The preparation method of chain laminated film.
Background technology
Laminated film, composite film, the material different by two or more passes through compounded thin film,
It is mainly used in functional material.By compound, it is possible to obtain there is the material of each homogenous material bulk properties, make
Base material mainly have plastic sheeting (such as polythene PE, polypropylene PP, polystyrene, polyvinylchloride
With polyester PET etc.), cellophane, paper and metal forming Al etc..The compound of base material can use extrusion compound
Method or carry out gluing compound by means of adhesive.Binding agent be the most of binding agent of sintetics be bi-component
The chemical reaction of polyurethane (PU) binding agent adhesion process make binding agent solidify.Binding agent at substrate surface
Mainly one physical process only have sub-fraction be chemical process at this moment binding agent composition with in plastic sheeting
Members bound solidify together and further.If thin film has been printed that in adhesion process
Binding agent and ink to meet more requirement.Most basic requirement is that the nexine before compound to have very well
Attachment fastness and be dried thoroughly.This means, in printing, film is not allow for dissolvent residual.But
The binder of ink often remains solvent or ethanol.For this reason, the performance of binding agent is necessary
Want to combine with free radical (-OH base).Otherwise binding agent and firming agent are understood self generation conglutination reaction thus are lost
The characteristic that should have.Such as in recombination process, thin film has been printed with PVB ink, remains in ink
Different atmosphere hydrochlorate, the chemical base-NCO of this salt can be combined with the free radical-OH of ethanol and water and react.No
Residual causes binding agent to be not sufficiently reacted.Come subsequently is exactly a not enough solidification and adhesion strength.?
In binding agent, the solvent type binding agent solvent-free binding agent this kind of with UV binding agent is distinguishing.
Solvent type binding agent needs a baking oven to make solvent volatilize away.When using UV binding agent, UV light passes
Thin film arrives binding agent makes plastering agent condense together.At present, in the preparation of some inorganic non-metallic thin film also
Use laminated film technology of preparing, reach the raising of photoelectric comprehensive performance.
At present, in MEMS, shape memory alloy actuator response frequency is low and deflection is little.Therefore, pass through
The present invention can prepare a kind of response frequency height in MEMS field, deflection of can being applied to and greatly and can realize remote
The Fe having orientation of journey remote control deformation3O4Nano chain/SBS/LLDPE magnetic control shape memory laminated film.
Summary of the invention
It is an object of the invention to provide a kind of based on MEMS orientation Fe3O4The preparation of nano chain laminated film
Method, it is intended to solve the problem that in MEMS, shape memory alloy actuator response frequency is low and deflection is little.
The present invention is achieved in that a kind of based on MEMS orientation Fe3O4The preparation of nano chain laminated film
Method, described based on MEMS orientation Fe3O4The preparation method of nano chain laminated film comprises the following steps:
Step one, solution full-boiled process synthesizing one-dimensional permanent magnetism Fe3O4Nano chain, with 1.56gFeCl3·6H2O and
2.72gFeSO4·7H2O is raw material, in hydrothermal reaction kettle, uses highly basic (NaAc) solution as reaction
Medium, is heated to 80 DEG C to reaction system, makes to produce in reactor the environment reaction 10h of High Temperature High Pressure, enters
And synthesize single dispersing Fe3O4Nano microsphere；By externally-applied magnetic field by Fe3O4Nano microsphere enters according to magnetic direction
Row arrangement, (mass ratio, in second dissolved with the dichloromethane solution of caprolactone diol and cross-linking agent then to use 35g
Esterdiol: DCP=100: 0.5～100: 2.5) carry out polyreaction (reaction condition: according to difference at microsphere surface
Ratio weighs esterdiol and DCP in second, it is dissolved completely in respectively in 20ml dichloromethane；Then with note
DCP solution is slowly injected in the second lactone glycol solution system of stirring by emitter, after it all adds again
With the ultrasonic mixed solution of ultrasonic dispersers 10 minutes, and it is placed on ventilating kitchen solvent flashing, is put the most again
It is completely dried to vacuum drying oven), by Fe under induced by magnetic field3O4Microsphere is self-assembled into one-dimensional Fe3O4Nano chain；
Step 2, Fe3O4Nano chain uniform dispersing method in blend solution, is 4.5～18% by mass fraction
Fe3O4Nano chain joins in the toluene solution being dissolved with SBS/LLDPE blend, in the condition of ice bath
Stir under (0 DEG C) and disperse；
Step 3, the first one-step forming of laminated film, use the method for spin-coating method film forming tentatively to be made by solution thin
The shape of film, after utilizing sol evenning machine suction piece, is added to solution on base plate, utilizes centrifugal force to open even for solution,
Controlled the thickness of solution by the rotating speed and time controlling sol evenning machine, prepare laminated film and (use substrate
It is 4 × 4cm2Ito glass sheet, during film, first spin coating 10s under 600r/min, then at 3000r/min
Operating 30s, is first dried 1h at 60 DEG C, repeats spin coating two-layer, obtains required sample).
Another object of the present invention is to provide a kind of described based on MEMS orientation Fe3O4Nano chain THIN COMPOSITE
Nano chain laminated film prepared by the preparation method of the film application in MEMS microactrator.
Another object of the present invention is to provide a kind of described based on MEMS orientation Fe3O4Nano chain THIN COMPOSITE
Nano chain laminated film prepared by the preparation method of the film application in MEMS microdrive.
What the present invention provided is orientated Fe based on MEMS3O4The preparation method of nano chain laminated film, Ke Yijie
The deflection closing shape-memory polymer is big, easy to process and magnetically controlled shape memory material fast response time
Advantage, designs and prepares and a kind of respond the magnetic control shape memory polymer thin fast, deflection is big and deformation is controlled
Membrane material can efficiently solve current shape-memory material bottleneck problem in MEMS, response time
＜ 10ms, deflection is up to 300% and deformation is accurately controlled within 1%, have important researching value with
Engineering significance.
Accompanying drawing explanation
Fig. 1 be the embodiment of the present invention provide based on MEMS be orientated Fe3O4The preparation of nano chain laminated film
Method flow diagram.
Fig. 2 is the Fe that the embodiment of the present invention provides3O4Nano microsphere and Fe3O4The microscopic pattern signal of nano chain
Figure；
In figure: a, Fe3O4Nano microsphere；b、Fe3O4Nano chain.
Fig. 3 is the Fe that the embodiment of the present invention provides3O4The magnetic response curve signal of/SBS/LLDPE laminated film
Figure.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment,
The present invention is further elaborated.Should be appreciated that specific embodiment described herein is only in order to solve
Release the present invention, be not intended to limit the present invention.
Below in conjunction with the accompanying drawings the application principle of the present invention is explained in detail.
As it is shown in figure 1, the embodiment of the present invention based on MEMS be orientated Fe3O4The system of nano chain laminated film
Preparation Method comprises the following steps:
S101: solution full-boiled process synthesizing one-dimensional permanent magnetism Fe3O4Nano chain.With FeCl3·6H2O and FeSO4·7H2O
For raw material, in hydrothermal reaction kettle, use strong base solution as reaction medium, reaction system is heated, makes
Reactor produces the environment of High Temperature High Pressure, and then synthesis single dispersing Fe3O4Nano microsphere；Pass through externally-applied magnetic field
By Fe3O4Nano microsphere arranges according to magnetic direction, then uses caprolactone diol and cross-linking agent at microsphere
Surface carries out polyreaction, by Fe under induced by magnetic field3O4Microsphere is self-assembled into one-dimensional Fe3O4Nano chain；
S102:Fe3O4Nano chain uniform dispersing method in blend solution, by Fe3O4Nano chain joins
In solution, under conditions of ice bath, long agitation (more than 24h) disperses；
The preliminary forming technique of S103: laminated film, uses the method for spin-coating method film forming tentatively to be made by solution
The shape of thin film, after utilizing sol evenning machine suction piece, is added to solution on base plate, utilizes centrifugal force to open even for solution,
Controlled the thickness of solution by the rotating speed and time controlling sol evenning machine, prepare laminated film.
Below in conjunction with specific embodiment, the application principle of the present invention is further described.
Step one, solution full-boiled process synthesizing one-dimensional permanent magnetism Fe3O4Nano chain, with 1.56gFeCl3·6H2O and
2.72gFeSO4·7H2O is raw material, in hydrothermal reaction kettle, uses highly basic (NaAc) solution as reaction
Medium, is heated to 80 DEG C to reaction system, makes to produce in reactor the environment reaction 10h of High Temperature High Pressure, enters
And synthesize single dispersing Fe3O4Nano microsphere；By externally-applied magnetic field by Fe3O4Nano microsphere enters according to magnetic direction
Row arrangement, (mass ratio, in second dissolved with the dichloromethane solution of caprolactone diol and cross-linking agent then to use 35g
Esterdiol: DCP=100: 0.5～100: 2.5) carry out polyreaction (reaction condition: according to difference at microsphere surface
Ratio weighs esterdiol and DCP in second, it is dissolved completely in respectively in 20ml dichloromethane；Then with note
DCP solution is slowly injected in the second lactone glycol solution system of stirring by emitter, after it all adds again
With the ultrasonic mixed solution of ultrasonic dispersers 10 minutes, and it is placed on ventilating kitchen solvent flashing, is put the most again
It is completely dried to vacuum drying oven), by Fe under induced by magnetic field3O4Microsphere is self-assembled into one-dimensional Fe3O4Nano chain；
Step 2, Fe3O4Nano chain uniform dispersing method in blend solution, is 4.5～18% by mass fraction
Fe3O4Nano chain joins in the toluene solution being dissolved with SBS/LLDPE blend, in the condition of ice bath
Stir under (0 DEG C) and disperse；
Step 3, the first one-step forming of laminated film, use the method for spin-coating method film forming tentatively to be made by solution thin
The shape of film, after utilizing sol evenning machine suction piece, is added to solution on base plate, utilizes centrifugal force to open even for solution,
Controlled the thickness of solution by the rotating speed and time controlling sol evenning machine, prepare laminated film and (use substrate
It is 4 × 4cm2Ito glass sheet, during film, first spin coating 10s under 600r/min, then at 3000r/min
Operating 30s, is first dried 1h at 60 DEG C, repeats spin coating two-layer, obtains required sample).
The Fe of the embodiment of the present invention3O4Nano chain orientation controlling technology and have orientation Fe3O4Nano chain
The preparation of/SBS/LLDPE composite, has orientation Fe3O4The system of nano chain/SBS/LLDPE laminated film
Standby flow chart is as shown in Figure 1；By applying the effect in magnetic field, to Fe3O4Nano chain carries out tropism control, system
Have the Fe of orientation3O4Nano chain/SBS/LLDPE laminated film, inquires into Fe3O4The orientation of nano chain is to multiple
Close the mechanism of action of the magnetic control shape memory performance of thin film.
Below in conjunction with the accompanying drawings the application effect of the present invention is explained in detail.
Fe3O4Nano microsphere and Fe3O4The microscopic pattern of nano chain is as shown in Figure 2.It can be seen that
Prepared Fe3O4Nanoparticle is spherical, and its particle diameter is about 400nm and distribution is narrower, Fe3O4
Nano chain is bar-shaped and is closely sized to.
Fe3O4The magnetism testing of/SBS/LLDPE laminated film；Fig. 3 Fe3O4/ SBS/LLDPE THIN COMPOSITE
The magnetic response curve of film；From figure 3, it can be seen that Fe prepared by the present invention3O4/ SBS/LLDPE THIN COMPOSITE
The magnetic response type of film is up to 81emu/g, and this illustrates Fe3O4/ SBS/LLDPE laminated film has preferable magnetic
Control shape memory effect.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this
Any amendment, equivalent and the improvement etc. made within bright spirit and principle, should be included in the present invention
Protection domain within.
Claims (8)
1. one kind is orientated Fe based on MEMS3O4The preparation method of nano chain laminated film, it is characterised in that
Described based on MEMS orientation Fe3O4The preparation method of nano chain laminated film comprises the following steps:
Step one, solution full-boiled process synthesizing one-dimensional permanent magnetism Fe3O4Nano chain, with FeCl3·6H2O and FeSO4·7H2O
For raw material, in hydrothermal reaction kettle, use strong base solution as reaction medium, reaction system is heated, makes
Reactor produces the environment of High Temperature High Pressure, and then synthesis single dispersing Fe3O4Nano microsphere；Pass through externally-applied magnetic field
By Fe3O4Nano microsphere arranges according to magnetic direction, then uses caprolactone diol and cross-linking agent at microsphere
Surface carries out polyreaction, by Fe under induced by magnetic field3O4Microsphere is self-assembled into one-dimensional Fe3O4Nano chain；
Step 2, Fe3O4Nano chain uniform dispersing method in SBS/LLDPE blend solution, by Fe3O4
Nano chain joins in solution, stirs and disperse under conditions of ice bath；
Step 3, the first one-step forming of laminated film, use the method for spin-coating method film forming tentatively to be made by solution thin
The shape of film, after utilizing sol evenning machine suction piece, is added to solution on base plate, utilizes centrifugal force to open even for solution,
Controlled the thickness of solution by the rotating speed and time controlling sol evenning machine, prepare laminated film.
2. it is orientated Fe based on MEMS as claimed in claim 13O4The preparation method of nano chain laminated film,
It is characterized in that, in step one, with 1.56gFeCl3·6H2O and 2.72gFeSO4·7H2O is raw material, at water
In thermal response still, use highly basic NaAc solution as reaction medium, reaction system is heated to 80 DEG C, makes
Reactor produces the environment reaction 10h of High Temperature High Pressure, and then synthesis single dispersing Fe3O4Nano microsphere.
3. it is orientated Fe based on MEMS as claimed in claim 13O4The preparation method of nano chain laminated film,
It is characterized in that, in step one, cross-linking agent is dichloromethane solution, and quality is than esterdiol in second: peroxidating
Diisopropylbenzene (DIPB)=100: 0.5～100: 2.5.
4. it is orientated Fe based on MEMS as claimed in claim 13O4The preparation method of nano chain laminated film,
It is characterized in that, in step one, the reaction condition of polyreaction: weigh esterdiol in second according to different proportion
And DCP, it is dissolved completely in 20ml dichloromethane respectively；Then with syringe, DCP solution is delayed
Slowly it is injected in the second lactone glycol solution system of stirring, ultrasonic with ultrasonic dispersers again after it all adds
Mixed solution 10 minutes, and it is placed on ventilating kitchen solvent flashing, put it to vacuum drying oven more completely dry
Dry.
5. it is orientated Fe based on MEMS as claimed in claim 13O4The preparation method of nano chain laminated film,
It is characterized in that, in step 2, by the Fe that mass fraction is 4.5～18%3O4Nano chain joins and is dissolved with
In the toluene solution of SBS/LLDPE blend, stir at the condition 0 DEG C of ice bath and disperse.
6. it is orientated Fe based on MEMS as claimed in claim 13O4The preparation method of nano chain laminated film,
It is characterized in that, in step 3, prepare laminated film and use substrate to be 4 × 4cm2Ito glass sheet, be coated with
During film, first spin coating 10s under 600r/min, then at 3000r/min operating 30s, be first dried at 60 DEG C
1h, repeats spin coating two-layer, obtains required sample.
7. one kind is orientated Fe based on MEMS as described in claim 1-6 any one3O4Nano chain THIN COMPOSITE
Nano chain laminated film prepared by the preparation method of the film application in MEMS microactrator.
8. one kind is orientated Fe based on MEMS as described in claim 1-6 any one3O4Nano chain THIN COMPOSITE
Nano chain laminated film prepared by the preparation method of the film application in MEMS microdrive.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110985358A (en) * | 2019-12-17 | 2020-04-10 | 西安电子科技大学 | Micropump driven by magnetic control SMP composite film |
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| CN102417567A (en) * | 2011-11-17 | 2012-04-18 | 西北工业大学 | Preparation method for one-dimensional magnetic thermo-sensitivity nanochain |
| CN103112904A (en) * | 2013-02-25 | 2013-05-22 | 哈尔滨理工大学 | Preparation method of nano Fe3O4 powder for preparation of nano dielectric medium through compounding with polyethylene |
| CN104672485A (en) * | 2015-02-13 | 2015-06-03 | 华中科技大学 | Photonic crystal thin film as well as preparation method and application thereof |
| CN104744713A (en) * | 2015-03-06 | 2015-07-01 | 西安理工大学 | Preparation method of polyvinyl alcohol-oxidized graphite-Fe3O4 composite film |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110985358A (en) * | 2019-12-17 | 2020-04-10 | 西安电子科技大学 | Micropump driven by magnetic control SMP composite film |
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