CN109632724A - A kind of real-time monitoring particle method of degree of orientation off field outside - Google Patents

A kind of real-time monitoring particle method of degree of orientation off field outside Download PDF

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Publication number
CN109632724A
CN109632724A CN201811518343.1A CN201811518343A CN109632724A CN 109632724 A CN109632724 A CN 109632724A CN 201811518343 A CN201811518343 A CN 201811518343A CN 109632724 A CN109632724 A CN 109632724A
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CN
China
Prior art keywords
particle
electric field
orientation
light transmittance
degree
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Pending
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CN201811518343.1A
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Chinese (zh)
Inventor
陈玉伟
张建明
刘玉红
王羽佳
杨吉颖
张白浪
李金博
段咏欣
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Qingdao University of Science and Technology
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Qingdao University of Science and Technology
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Priority to CN201811518343.1A priority Critical patent/CN109632724A/en
Publication of CN109632724A publication Critical patent/CN109632724A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/59Transmissivity
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00Characterised by the use 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; Derivatives of such polymers
    • C08J2383/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon

Abstract

The present invention provides a kind of methods of particle that can be monitored in real time in flowable media degree of orientation under the electric field.By the Combination Design of light transmittance detection device and electric field generation device, to realize the variation of light transmittance caused by the motion state of particle in real-time monitoring flowable media, by the variation of light transmittance, it can accurately infer whether particle is orientated in the medium.

Description

A kind of real-time monitoring particle method of degree of orientation off field outside
[technical field]
The present invention relates to composite material film technical field, in particular to outfield auxiliary prepares anisotropic composite material film Monitoring technical field in process.
[background technique]
After particle filler orientations in a polymer matrix, the composite material of preparation has each to different in structure Property, to make composite material that there is anisotropic properties, such as optical property, mechanical performance, electric property and hot property.In recent years Come, induces particle orientations in flowable media to prepare ordered structural material as outfield force by electric field and obtain scientific work Author's studies and makes some progress extensively, such as: the Chinese invention patent of Patent No. CN102831992 utilizes electricity Field induction montmorillonite oriented in molten polyethylene.
The mechanism arranged with the development of technology with the accumulation of experience, people by analysis electric field induced orientation, Yi Ji The movement mechanism of particle of different shapes under electric field action, and combine the influence factor of electric field induced orientation arrangement, it is believed that particle Orientations under electric field action are the processes that electric field polarization effect and the warm-up movement of particle compete, and grasp and utilize electric field Particle orientation technology is induced, a series of composite materials with property and effect are successfully prepared.These composite materials are in reality In the application of border, because having anisotropic advantage to be widely popularized.BJ University of Aeronautics & Astronautics Liu Mingjie teaches [1] etc. People reviews the latest Progress with height-oriented nano composite structure hydrogel, compared to the hydrogel not being orientated, Be greatly improved on abrasion resistance properties in conjunction with the hydrogel of height-oriented structure, and with tissue more phase Seemingly, therefore at present orientations are just pushing Nanometer composite hydrogel to anisotropic biologic soft tissue Materials.Phase The similar intelligent macromolecule material [2] popular there are also the past few years, this material are made in uniform magnetic field or electric field, Due to producing dipole in preparation process, make to interact to form the end to end chain of particle there are extremely strong between particle Shape structure, it is whole to be arranged in the material in " one " shape, generate anisotropy.Material obtained can be in magnetic compared to common material It is bent in field, electric field, response electric and magnetic fields effect meets needs in real life.
At this stage, numerous for this kind of material surface pattern research method, such as: scanning electron microscope, transmission electron microscope, atomic force Microscope etc., but these methods require that first preparing sample then characterizes sample, can not supervise in real time in actually preparation It surveys particle and is aligned degree in flowable media by electric field induction, there are inconveniences in production application, especially exist In plant produced, due to can not real-time monitoring particle orientation degree, cause raw particles largely to waste, preparation time extend etc. ask Topic, hinders the development and application of special construction material to a certain extent.
It is learnt by light reflection principle, incident light irradiation is applied to the particle of random dispersion in the base, light is very big Stopped in degree by particle and generate reflection, the light transmittance of material is caused to reduce.But after particle orientation arrangement, light can be The probability that differently- oriented directivity is reflected reduces, and the light transmittance enhancing of material, early in 1998, Bianca etc. [3] just utilized electric light skill Art obtains scatter spectra image of the gold particle under different dispersities, and has studied its particle orientation situation.This technology is special Niche is taken in this theory, the anisotropy shown using orientations material in optical property by real-time monitoring Characterize the size of material degree of orientation indirectly to the variation of direction material transmissivity.Actual experiment proves: when light transmittance is high, sample Particle orientation degree is high, conversely, sample particle degree of orientation is then low, meanwhile, it is orientated by light transmittance mutation analysis sample particle Degree acquired results are no different with actual conditions obtained by micro- sem observation, and accuracy and reliability with higher can actually ground Study carefully and applies and promote in preparing.
Since particle can carry out orientations under external field evoked in flowable media to obtain ordered structure, This technology has certain development latent in the especially nanocomposite preparation field of the field of compound material with special construction Power, and this composite material has pushed medicament preparation, fine chemistry industry production and the innovation and development of daily chemical product.In conjunction with light transmission The relationship of rate and material degree of orientation, this technology patent disclose particle orientation degree in above-mentioned real-time monitoring flowable media Method, the specific steps are as follows:
(1) design installation electric field or induced by magnetic field experimental provision, and it is equipped with light transmittance detection device and sample cell.
(2) open control device of electric field, under the microscope by extra electric field in sample cell be in flowable media in grain Son carries out Induction experiments, the variation of real-time detection light transmittance.
(3) light transmittance mutation analysis is combined to obtain the real-time degree of orientation of sample particle.
(4) acquired results are compared with obtained by micro- sem observation, and research is discussed
Investigation is learnt, prepares composite material using the method that external field evoked particle orientation arranges, and is only at present preliminary Stage, but this direction has received the attention of various countries scientific worker, has especially started in recent years and has probed into carbon nanotube in electricity The upsurge of arrangement off field.Therefore the particle in real-time monitoring flowable media described in this technology patent is orientated off field outside The method of degree can be widely applied in scientific research and R&D process to the structure of anisotropic composite material preparation process point Analysis, technological evaluation etc. push the special construction Materials of orientations.
[summary of the invention]
The object of the present invention is to provide a kind of particle that can be monitored in real time in flowable media degree of orientations off field outside Method, effectively solve particle by external field evoked front and back degree of orientation characterization problems.
The technical scheme is that the anisotropy showed using oriented material in optical property, probes into obtain one kind Flowable Jie can be monitored in real time.
Particle in the matter method of degree of orientation off field outside, it is characterised in that: design electric field induction particle orientation experiment Device, and it is equipped with light transmittance detection device.Then orientation Induction experiments are carried out in particle in flowable media, it is real in the process When detection light transmittance variation, eventually by orientation fore-and-aft architecture light transmittance mutation analysis particle degree of orientation.
The advantage of the invention is that the method for the variation characterization degree of orientation by light transmittance being previously mentioned, it can be by taking The variation before electric field induces particle orientation with degree of orientation after orientation is distinguished with the variation of system light transmittance after orientation forward.Nothing Need to be by complicated equipment, operating process is simple, and confirms through micro- sem observation sample, as a result reliably.
[Detailed description of the invention]
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with attached drawing to the present invention do into The detailed description of one step, in which:
Fig. 1 is the front view of experimental provision of the present invention
Fig. 2 is that degree of orientation influences schematic diagram to material transmissivity
Fig. 3 is light transmittance with sample orientation change curve
Fig. 4 is orientation and non-oriented sample drawing
Fig. 5 is the optical microscope of orientation with non-oriented sample section
[specific embodiment]
Hereinafter reference will be made to the drawings, and a preferred embodiment of the present invention will be described in detail.It should be appreciated that preferred embodiment Only for illustrating the present invention, rather than limiting the scope of protection of the present invention.
In Fig. 1,1-ITO electro-conductive glass top electrode, electrode under 2-ITO electro-conductive glass, 3- light transmittance tester light receiver End, 4- light transmittance tester light issuing side, 5- light transmittance tester transmitting light, 6- light transmittance tester display control end, 7- sample accommodates pond, 8- sample, 9- electric field controls equipment.
The aligning device includes the top electrode 1 served as by ITO electro-conductive glass and lower electrode 2, and ITO conductive layer is located at top electrode Lower surface, the upper surface of lower electrode, it is the glass slit institute structure by being affixed on lower electrode surface that sample between the two, which accommodates pond 7, At rectangular receiving pond, after energization accommodate pond in contained sample 8 be then placed in uniform electric field.
Electric field controls equipment 9 is made of high-voltage amplifier, signal controller and oscillograph three parts, by controlling high pressure Amplifier and signal controller obtain required electric field strength, frequency, waveform, pass through oscillograph real-time monitoring high voltage amplifier Virtual voltage, the waveform, frequency of device output end (being applied to upper/lower electrode).
Embodiment 1.
Using dimethyl silicone polymer (PDMS) as flowable media, 325 mesh graphite as orientation particle, by graphite with Ratio of the PDMS with mass ratio for 1:200, which is uniformly mixed, is made graphite and PDMS mixed liquor.Using ito glass as parallel transparent Electrode, and electric field generating device is connected, including high-voltage amplifier, signal generator and oscillograph.Mixed liquor is placed in transparent Between electrode, transparent electrode is placed in light transmittance tester using grain-clamping table.Setting alternating current voltage is 400V, and frequency is 100Hz powers on, and then tends to after light transmittance rapid increase in ten seconds record light transmittance changes, detection process Stablize, also confirms that powering on rear degree of orientation increases rapidly, and reach highest over time.It is solid by being added in mixed liquor Agent, and make curing agent and PDMS mass ratio 1:10, heating the sample to 90 DEG C of maintenance 30min can be such that sample solidifies, and pass through Orientation and non-oriented sample is made in the method, and by comparing the light transmittance of two kinds of samples, orientation sample is apparently higher than non-oriented sample Product also demonstrate the presence of the orientation texture of particle in orientation sample eventually by micro- sem observation.
Embodiment 2.
Specific experiment scheme is similar to Example 1, is not uniquely both to be orientated voltage in embodiment 2 to control as 800V.Voltage Raising can lead to particle degree of orientation increase and speed of orientation quickening.

Claims (7)

1. a kind of method of particle in real-time monitoring flowable media degree of orientation under the electric field, it is characterised in that this method packet Include following steps:
1) it disperses uniform particle to be orientated in selected flowable media;
2) electric field induction particle orientation device is built, while combining light transmittance monitoring device;
3) apply electric field, light transmittance variation is monitored by light transmittance detector.
2. monitoring method according to claim 1, it is characterised in that: the orientation particle can be nanoscale to grade Most filler grains, particle shape can be bar-like, sheet, spherical or other irregular arbitrary shapes.
3. monitoring method according to claim 1, it is characterised in that: the flowable media refers to that particle is dispersed therein Liquid, gas or jelly can be can be with free-moving medium, the medium.
4. monitoring method according to claim 1, it is characterised in that: the electric field induction particle orientation device includes electric field Control equipment, power-on and power-off pole plate, sample cell.
5. monitoring method according to claim 1, it is characterised in that: the light transmittance monitoring device can be by upper/lower electrode And sample cell is placed between light issuing side and light receiver end, is changed by sample transmittance, indirect judgement sample particle Degree of orientation.
6. electric field according to claim 4 induces particle orientation device, it is characterised in that: the electric field controls equipment be by Signal controller, high-voltage amplifier and oscillograph three parts are constituted.Extra electric field can be DC voltage or alternating voltage, voltage And frequency is adjustable.
7. electric field according to claim 4 induces particle orientation device, it is characterised in that: the sample cell is transparent material The receiving pond of the flowable liquids of composition, sample cell is placed between upper/lower electrode in detection process.
CN201811518343.1A 2018-12-12 2018-12-12 A kind of real-time monitoring particle method of degree of orientation off field outside Pending CN109632724A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110568689A (en) * 2019-09-05 2019-12-13 浙江大学 Method for regulating orientation of liquid crystal element in colloidal liquid crystal
CN113390950A (en) * 2021-05-28 2021-09-14 杭州电子科技大学 Portable thermal-electric coupling induced polymer forming experimental device and experimental method thereof

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JP3979500B2 (en) * 2003-11-21 2007-09-19 独立行政法人科学技術振興機構 Organic microcrystalline alignment dispersion, polarized fluorescent material, and production method thereof
CN1658029A (en) * 2004-01-15 2005-08-24 夏普株式会社 Display element and display device
CN1649094A (en) * 2004-12-28 2005-08-03 东南大学 External electric field induced orientation sedimentation method for preparing nano gap
CN102627835A (en) * 2012-03-30 2012-08-08 富维薄膜(山东)有限公司 Addition type composite particle for polyester film, preparation method of addition type composite particle and optical polyester film added with composite particle
CN102831992A (en) * 2012-08-13 2012-12-19 重庆大学 Device and method for inducing orientation arrangement of montmorillonoid in polyethylene by using electric field
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110568689A (en) * 2019-09-05 2019-12-13 浙江大学 Method for regulating orientation of liquid crystal element in colloidal liquid crystal
CN113390950A (en) * 2021-05-28 2021-09-14 杭州电子科技大学 Portable thermal-electric coupling induced polymer forming experimental device and experimental method thereof
CN113390950B (en) * 2021-05-28 2023-08-25 杭州电子科技大学 Portable thermal-electric coupling induced polymer molding experimental device and experimental method thereof

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