CN102590047A - Dispersion measurement method of inorganic nano-particle composite polyimide film raw material - Google Patents
Dispersion measurement method of inorganic nano-particle composite polyimide film raw material Download PDFInfo
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Abstract
The invention relates to a dispersion measurement method of an inorganic nano-particle composite polyimide film raw material, comprising the following steps of: (1) placing a proper amount of a sample into a measurement container and then placing a metal plate electrode into the measurement container; (2) applying an alternative current voltage on two electrode plates, gradually increasing the voltage amplitude and recording a breakdown voltage measurement value; ( 3) comparing the measurement value with the standard value and analyzing; and (4) analyzing the measurement result, wherein the closer the measurement value and the standard value are, the more uniform the dispersion of the nano particles in the sample is. The time is saved, the dispersion is directly measured free from the limit of various dispersion stability mechanisms, the experiment device is simple, the measurement operation is convenient, and the experiment result is visual and accurate. The dispersion measurement method is mainly used in the technical field of the electronic insulation.
Description
Technical field
The present invention relates to a kind of dispersed detection method of inorganic nanoparticles, relate to the dispersed detection method of a kind of inorganic nanoparticles compound polyimide film raw material or rather, belong to the electric insulation technical field.
Background technology
In recent years, the usable range of variable-frequency motor was more and more wider.Efficiently; Energy-conservation; Being easy to advantage such as control makes variable-frequency motor have much the DC speed regulation trend that substitutes in metallurgy, lifting, all fields of locomotive traction; Since particularly igbt (IGBT) comes out, brought up to about 10-20K about the 1-2K of carrier frequency during, electrical machine insulation has been brought outstanding problem from bipolar transistor (GTR).A large amount of momentary pulse peak voltages are applied in turn-to-turn (the particularly first circle) insulation, cause the electrical machine insulation premature damage, have a strong impact on running reliability of motor.In view of this, U.S.'s NEMA standard has been done corresponding change, to the examination of general service motor by MG1; Part30 (peak value 1000V, 2us rise time) changes MG1, Part31 (peak value 1600V into; 0.1us the rise time), improved requirement to the anti-high-frequency impulse of motor turn-to-turn insulation.
In the electric insulation technical field, organic film kind commonly used is a lot, mainly contains polyester (polyethylene terephthalate) film, polypropylene film, polyvinyl chloride film, polyethylene film, plasticon, Kapton etc.Wherein, polyimide (PI) is the highest macromolecular material of temperature classification of widespread use in a kind of industry, and the excellent performance that it at high temperature possesses can compare favourably with some metal.In addition, it also has excellent chemical stability, toughness, wearing quality, anti-flammability, electrical insulating property and other mechanical property.Above excellent comprehensive performance makes polyimide be known as to surmount the material in epoch to be the first-selection of organic film in the electric insulation technical field.
Along with the develop rapidly of modernization industry, also increasingly high to the requirement of material property.But generally contain phenyl ring and imide ring structure on the PI molecular backbone; Because electron polarization and crystallinity; Cause PI to exist between stronger strand and act on, cause that the PI strand is tightly packed, thereby cause tangible water absorptivity of PI and thermal expansivity; A little less than causing PI film corona resistance very, this has limited its application under high temperature and accurate state.For satisfying the wide market demands of variable-frequency motor, the electromagnetic wire industry must be made great efforts exploitation and adapted to high-frequency pulse voltage, the electromagnetic wire of anti-corona.As far as the high-pressure frequency-conversion motor, must develop the Kapton (CRPI film) of anti-corona, make winding wire with it, to solve the not weakness of anti-corona of common PI film.
Inorganic nano-particle has all shown bigger advantage owing to have unique character such as " size effect ", " interfacial effect " and " tunnel effect " at the aspects such as heat resistance, mechanical property and dimensional stability that improve material.Therefore study inorganic nano-particle (SiO
2, TiO
2, SiO
2/ TiO
2, Al
2O
3Deng) have important significance for theories and using value in the application of modified polyimide (PI).The corona resistance of polyimide/inorganic nano compound substance and physical strength and toughness all improve significantly than pure polyimide, and because the compound material that makes of the nanoscale of the two obtains outstanding performance.
At present, the preparation method of polyimide/inorganic nano compound substance mainly contains sol-gel (Sol-gel) method, dispersion copolymerization method on the throne and graft process.
The polyimide/inorganic nano compound substance is widely used: can be used as gas separation membrane, sensitization compound substance, microelectronic component, wrappage, also can be used for friction field.
Though; Nano particle particularly all improves significantly and improves in aspects such as thermal behavior, mechanical property and permeability the performance of PI; But the inorganic nano-particle in the PI/ inorganic nano composite material does not reach whole nanoscale yet to be disperseed, just certain a part of nano-dispersed.This is because the size of nano particle is little; There are a large amount of unsaturated links in the surface, and surfactivity is very big, belongs to thermodynamic unstable system; Particle coalescence, agglomeration very easily take place in the preparation process or in the last handling process; Form second particle, make particle diameter become big, the peculiar function that finally loses nano particle in use and possessed.And the dispersion stabilization of nano particle in inorganic nanoparticles compound polyimide film raw material directly determining the corona-resistance property of inorganic nanoparticles compound polyimide film.Therefore, the dispersion process of research nano particle in medium prevents nanoparticle agglomerates, and the inorganic nanoparticles compound polyimide film raw material that obtains the nano particle good dispersion is most important.
The reunion of nano particle can be divided into two kinds: soft-agglomerated and hard aggregation.Soft-agglomerated mainly is by due to intergranular electrostatic force and the Van der Waals force, can eliminate through some chemical actions or the mode that applies mechanical energy because acting force is more weak.The reason that hard aggregation forms also have chemical b `, so hard agglomeration is survivable except electrostatic force and Van der Waals force, need take some special methods to control.In the process of preparation nano particle, if do not adopt the dispersion measure, particle agglomeration will be very serious, can not reach the basic demand of nanometer powder, realize not the specific function of nanometer powder.Therefore the reunion control of studying nano particle is very important to the nanometer powder preparation.
The reason that causes nanoparticle agglomerates is a lot, and concluding gets up mainly is because the special surface structure that nano particle had is existing the interaction energy-nanometer interaction energy (F that is different between conventional particle (particle) between particle
n), the nanometer interaction energy is the internal factor that nano particle be prone to be reunited, and obtain that good dispersion, particle diameter are little, the nano particle of narrow diameter distribution, must weaken or reduce the nanometer interaction energy.Pursue the proper method when nano particle carried out dispersion treatment, nano grain surface produces the solvation membrane interaction can (F
s), the electrostatic double layer electrostatic interaction can (F
r), the space protection interaction energy (F of polymkeric substance adsorbed layer
p) etc.In certain system, nano particle should be the equilibrium state that is in these several kinds of interaction energies, works as F
x＞F
s+ F
r+ F
pThe time, nano particle is prone to reunite, and works as F
m＜F
s+ F
r+ F
pThe time, nano particle is prone to disperse.In addition, intermolecular force, electrostatic interaction, active high chemical bond (like hydrogen bond) also are the key factors that causes nanoparticle agglomerates usually, show more strongly in nano particle small-medium size effect and surface effect.Because intercoupling of the quantum tunneling effect of nano particle, electric charge transfer and interface atom makes nano particle very easily through the interface interaction take place and solid phase reaction is reunited.Because of its high surface energy and bigger contact interface, make speeding up of grain growth, thereby particle size is difficult to remain unchanged.Some nano particle is (like CaCO
3) because hydrolytic action, the surface is stronger alkalescence, hydroxyl property and water of coordination molecule, and they can pass through hydroxyl and the condensation of water of coordination molecule, generate hard aggregation.
The dispersion process of nano particle in liquid medium, the dispersion process of conventional granulates in liquid medium that can use for reference the comparative maturity that has proposed is theoretical.The dispersion process of conventional granulates in liquid medium is divided into 3 stages: wetting, dispersion and stable.Different with conventional granulates is; Nano particle is that size reaches nano level solid particle; So the dispersion process of nano particle in liquid medium also can be thought these 3 stages of branch: 1. wetting (nano particle is immersed in wetting in the liquid medium, belongs to and soaks) of nano particle; 2. the dispersion of nano particle or cracked (making bigger aggregation be separated into less nano particle) through external influence power; 3. nano particle stablizes (the assurance nano particle keeps long-term and evenly disperses in liquid phase, prevent that the nano particle that has disperseed from reassembling).
According to the difference of nanoparticulate dispersed method, can be divided into physics and disperse and chemical dispersion.
1. physics disperses
The physics process for dispersing mainly contains 3 kinds: mechanical raking dispersion, ultrasonic dispersing and high power treatment method are disperseed.
1) mechanical raking is disperseed
It is that a kind of simple physics is disperseed that mechanical raking is disperseed, and mainly is by mechanical energy such as extraneous shearing force or impacts, and nano particle is fully disperseed in medium.In fact; This is a very complicated dispersion process; Be through dispersed system being applied the physics that mechanical force causes material in the system, the series of chemical that chemical property changes and follows, reach the dispersion purpose, this special phenomena is referred to as mechanochemical effect.The concrete form that mechanical raking is disperseed has the dispersion of grinding, colloid mill dispersion, Ball milling, high-speed stirred etc.Under mechanical raking, the special surface structure of nano particle is easy to generate chemical reaction, is formed with organic compounds side chain or protective seam and makes nano particle more be prone to disperse.
2) ultrasonic dispersing
Ultrasonic dispersing is to reduce the effective ways of nanoparticle agglomerates, and it is relevant with cavitation that its mechanism of action is thought.The localized hyperthermia, high pressure or strong shock wave and the microjet etc. that utilize ultrasonic cavitation to produce, the nanometer interaction energy between nano particle of can weakening greatly prevents nanoparticle agglomerates effectively and makes it abundant dispersion.Ultrasound wave has vital role to synthetic, the degraded of polymkeric substance of compound, the dispersion of particulate matter, and bigger ultrasonic power can more effectively destroy intergranular reunion.But should avoid ultrasonic time to cross for a long time during ultrasonic dispersing and cause overheated because along with the rising of temperature, the probability of impact of particles also increases, and can further aggravate on the contrary to reunite.Therefore, should select the ultrasonic jitter time that suits.
3) the high power treatment method is disperseed
The high power treatment method is through the high energy particle effect, produces active site at nano grain surface, increases surfactivity, makes it be prone to other material generation chemical reactions or adheres to, and the nano grain surface modification is reached be prone to the purpose of disperseing.High energy particle comprises corona, ultraviolet light, microwave, plasma ray etc.
2. chemical dispersion
Chemical dispersion comes down to utilize surface chemistry method adding surface conditioning agent to realize the method for disperseing.Can change the surface structure and the state of nano particle through carrying out chemical reaction between nano grain surface and the treating agent, reach the purpose of surface modification; In addition, also can change the surface charge distribution of particle, produce electrostatic stabilization and sterically hindered stabilization and strengthen dispersion effect through dispersant adsorption.
1) coupling agent method
Coupling agent has the both sexes structure, a part of group in its molecule can with the various functional group reactionses of particle surface, form strong chemical bonding, some chemical reaction or physics can take place with organic polymer and twine in another part group.Particle after coupling agent treatment; Both suppressed the reunion of particle itself; Strengthen the solubility of nano particle in organic media again, it can be dispersed in the organic matrix preferably, increased particles filled amount; Thereby improve the combination property of goods, particularly tensile strength, impact strength, pliability and flexural strength.
2) esterification
Metal oxide is called esterification with the reaction of alcohol.With esterification nano grain surface is modified, importantly made the surface of original hydrophilic oleophobic become the surface of oleophilic drainage, the modification of this function of surface is very important in practical application.The esterification surface modification is that faintly acid is the most effective with neutral nano particle for the surface.
3) spreading agent disperses
Select one or more suitable spreading agents to improve the dispersiveness of suspended matter, improve its stability and rheological.Spreading agent commonly used mainly contains inorganic electrolyte or the inorganic polymer (like sodium silicate, sodium hexametaphosphate etc.) of the surfactant of being made up of lipophilic group and hydrophilic group (like LCFA, cetyl trimethyl ammonium bromide (CTAB) etc.), little relative molecular mass, the polymkeric substance and the polyelectrolyte (like gelatin, CMC, poly-methyl acrylate, polyethyleneimine etc.) of relative molecular mass greatly.But it should be noted that when the quantity not sufficient that adds people's spreading agent or when excessive, possibly cause flocculation.When therefore using spreading agent to disperse, must control its consumption.
Interaction potential energy total between the particle can be expressed as:
V
T＝V
WA+V
ER+V
SR
In the formula, V
WABe Van der Waals force potential energy; V
ERBe double electrode layer repulsion potential energy; V
SRScold potential energy for sterically hindered.
Hence one can see that, and the nanoparticulate dispersed stable mechanism mainly contains following three kinds:
1. electronic double layer repulsion theoretical (dlvo theory)
Dlvo theory mainly is to explain mechanism and the stable factor of influence that dispersed system is stable through the electrostatic double layer theory of particle.This theory is can form an adsorbed layer at particle surface having ignored macromolecule, has also ignored because polymkeric substance adsorbs simultaneously to produce a kind of new repulsion--set up under the situation of sterically hindered repulsion.This theory has disclosed the electrically charged and stability relationship of nano grain surface, and the pH value through reconciling solution or add method such as electrolytic solution increases the particle surface electric charge; Form electrostatic double layer; Increase through Zeta potential, make to produce the Coulomb repulsion effect between particle, realize the stable dispersion of particle.The stability of system mainly is can realize that expression formula is following with the balance of Van der Waals force ability through electronic double layer repulsion
V
T＝V
WA+V
ER
In the formula, V
TBe the total potential energy of two particle; V
WABe Van der Waals force potential energy; V
ERBe double electrode layer repulsion potential energy.
2. sterically hindered stable mechanism
The electronic double layer repulsion theory can not be used for explaining the stability of the colloidal system of superpolymer or non-particle surface activating agent.For through adding the system of high molecular polymer, can explain with sterically hindered stable mechanism as spreading agent.High molecular polymer is adsorbed on the surface of nano particle; Form one deck polymer protective film, surrounded nano particle, stretch to the lyophily group in the water; And has a certain thickness; This shell has increased immediate distance between two particle, has reduced the interaction of Van der Waals force, thereby makes dispersed system be able to stablize.The particle that has adsorbed high molecular polymer will produce two kinds of situation when near each other: a kind of is that adsorbed layer is compressed and does not interpenetrate; Another kind is that adsorbed layer can interpenetrate, overlap each other.Both of these case all can cause maximum system energy to raise, and free energy increases.First kind of situation produces entropy repulsion potential energy owing to macromolecule loses structure entropy; Second kind of situation causes producing infiltration repulsion potential energy and mixes the repulsion potential energy because overlapping region concentration raises.Thereby, take place again to reunite with the ten minutes difficulty if adsorbed high molecular nano particle, thereby realized dispersion of nano-particles.
3. static steric hindrance stable mechanism
If electrostatic stabilization and space steric effect are combined, can play better stablizing effect.The static steric stabilization; Be that nanoparticle surface has been adsorbed the charged stronger polymer molecule layer of one deck; Charged polymer molecule layer both through itself with electrical charge rejection around particle, utilize again particle that steric effect prevents to do Brownian movement near, produce the stable composition effect.Wherein the electrostatic charge source is mainly the particle surface static charge, adds electrolyte and the high polyelectrolyte of anchoring group.Particle is when distance is far away, and electrostatic double layer produces repulsion, and static is leading; Particle when close together, sterically hindered prevention particle near.Spreading agent as the static steric. dispersion generally has: polyacrylamide, sodium polyacrylate, sodium alginate, ammonium alginate, wooden sodium carbonate, petroleum sodium sulfonate, polyacrylic acid acyl ammonium, hydrolysis ammonium acrylate, phosphoric acid fat, ethoxy compound etc.
The dispersion of nano particle in medium is the process of a dispersion and flocculation balance.Although physical method can better be realized the dispersion of nano particle in liquid phase medium,, owing to the intermolecular force effect, can assemble each other again between particle in case external influence power stops.And the employing chemical dispersion through changing particle surface character, changes particle and liquid phase medium, particle and intergranular interaction, and the repulsive force between enhanced granule is with producing the lasting effect that flocculation is reunited that suppresses.Therefore, in the real process, should physics dispersion and chemical dispersion be combined, separate reunion, keep stably dispersing,, obtain the strong inorganic nanoparticles compound polyimide film of corona resistance to reach better stably dispersing effect with chemical method with physical means.
Development along with the nano-dispersed technology will propose increasingly high requirement to the dispersion stabilization of nano particle in inorganic nanoparticles compound polyimide film raw material.How to judge the dispersion stabilization of nano particle in medium, just produced the appraisal procedure problem of dispersion stabilization.From present research, mainly contain sedimentation, granularity observation method, Zeta potential method and light transmittance ratio method etc.
1) sedimentation
The system of dispersion stabilization difference is the rapid sedimentation of flocculation of a formula more, and the interface of precipitum and upper clear supernate formation one clear Zha, reaches sedimentation equilibrium very soon.The settling velocity that dispersion stabilization is good is slow, and the particle of dispersed system from top to bottom is the disperse distribution of enrichment gradually, does not have tangible sediment.The concrete operations of sedimentation are: scattered dispersed system is poured in the graduated cylinder, left standstill, observe the volume or the height of precipitum.
Sedimentation can be used for studying the influence of each factor to liquid dispersion system dispersion effect, can react the dispersion stabilization of nano particle in liquid medium truly, and easy and simple to handle, is present the most frequently used and the most reliable a kind of method.Weak point is that the test period is long, might place 10d, one month even sedimentation does not take place half a year for the good dispersed system of dispersion stabilization.
2) granularity observation method
The granularity observation method is through the granularity of nano particle or the appraisal procedure a kind of commonly used of size distribution in the observation dispersed system.The dispersed system particle size that dispersion stabilization is good should be the size of a nano particle.Opposite granularity the greater explains that this dispersed system has reunion to a certain degree on the one hand; Its suffered gravity effect in dispersed system is bigger on the other hand, and settling velocity is accelerated, thereby has quickened the instability of system.At present, the method for measuring the nanoparticle granularity is a lot, and the useful transmission Electronic Speculum is observed the dispersion effect of nano particle, and also useful special particle-size analyzer is observed, also useful X ray particle size analyzer the granularity of particle in the dispersed system.
Concrete operations from present used granularity observation method; Granule size of measuring or size-grade distribution all are through handling the result that (like dilution) back is observed in the dispersed system; It is thus clear that this method not only can not directly be measured outside the size of nano particle in liquid medium; And it is limited to take a sample, and the result lacks statistical.
3) Zeta potential method
Nanoparticulate dispersed is in liquid medium, and particle surface has the net charge of some, and the opposite charges that attracts equivalent amount is around it, and the current potential of fixed layer and diffusion layer intersection slipping plane is a Zeta potential.The absolute value of Zeta potential is big more, and the electrostatic repulsion between the particle is preponderated, and is difficult for reuniting, and explains that dispersed system is stable; On the contrary, the absolute value of Zeta potential is more little, and the Van der Waals force between the particle is preponderated, and reunites easily, explains that the system dispersion stabilization is poor.Therefore, this method is exactly to assess the dispersion stabilization of dispersed system through the size of measuring the particle surface Zeta potential.Through measuring the Zeta potential of particle surface, can reflect the stability of dispersed system, to confirm suitable electrolyte and system pH, finally obtain the good dispersed system of dispersion stabilization.
Use the method for measuring Zeta potential to assess the dispersion stabilization of dispersed system, can draw test findings soon, this is the great advantage of this method.But this method is on the theoretical foundation of electrostatic stabilization mechanism, to set up, and the dispersed system of inapplicable sterically hindered stabiliser system has limitation.
4) light transmittance ratio method
This method is to utilize that nano particle has absorption to certain wavelength incident light in the dispersed system, and the size of its absorbance satisfies Lambert-Beer's law, that is: A=-logT=ε
mBC
sA is an absorbance in the formula, ε
mBe molar absorptivity, b is the thickness of sample cell, C
sBe the content of nano particle in the dispersed system, T is a transmittance.At ε
m, under the identical condition of b, the content C of negative logarithm of the transmittance of dispersed system and nano particle
sInversely proportional relation.Along with the increase of nano-particle content in the dispersed system, transmittance reduces, if transmittance no longer reduces, can think that dispersed system has reached the state of stably dispersing.That is to say that for different dispersed systems, under the same conditions, the dispersion stabilization of the little person's system of transmittance will be got well.Generally measure transmittance with spectrophotometer.
The advantage of this method is intuitively, saves time, but this method is a kind of appraisal procedure that puts forward according to Lambert-Beer's law, only is suitable for lean solution, and certain limitation is arranged, and is not the direct method of assessment dispersion stabilization equally.
Summary of the invention
The object of the present invention is to provide the dispersed detection method of a kind of inorganic nanoparticles compound polyimide film raw material, overcome the shortcoming of the dispersed detection method of existing inorganic nanoparticles.
1. sedimentation need be poured scattered dispersed system in the graduated cylinder into, leaves standstill, and observes the volume or the height of precipitum.Its test period is long, and the dispersed system that dispersion stabilization is good might be placed 10 days, one month even sedimentation do not take place half a year.
2. the granularity observation method is granularity or the size distribution through nano particle in the observation dispersed system; Granule size that this method is measured or size-grade distribution all are through handling the result that (like dilution) back is observed in the dispersed system; Not only can not directly measure outside the size of nano particle in liquid medium; And it is limited to take a sample, and the result lacks statistical.
3. the Zeta potential method is on the theoretical foundation of electrostatic stabilization mechanism, to set up, and therefore the dispersed system of inapplicable sterically hindered stabiliser system also has limitation.
4. the transmittance rule puts forward according to Lambert-Beer's law, only is suitable for lean solution, and certain limitation is arranged, and is not the direct method of assessment dispersion stabilization equally.
The present invention detects the dispersion stabilization of nano particle in the inorganic nanoparticles compound polyimide film raw material through measuring the voltage breakdown of inorganic nanoparticles compound polyimide film raw material; Obtain to have the inorganic nanoparticles compound polyimide film raw material of good dispersion with this,, satisfied requirement the anti-high-frequency impulse of variable-frequency motor turn-to-turn insulation in order to the good inorganic nanoparticles compound polyimide film of preparation corona-resistance property.
The present invention is through being achieved through following technical scheme.
The detection method that a kind of inorganic nanoparticles compound polyimide film raw material is dispersed has following steps:
(1) gets inorganic nano combined Kapton raw material to be measured and pour in the detection receptacle, container is filled, and go down except that bubble, in this sample, put into the metal plate electrode again in vacuum environment;
(2) apply the 0-10kV alternating voltage to two-plate, begin to increase voltage magnitude by 0.5kV/s speed from 0kV, the inorganic nanoparticles compound polyimide film raw material discharge breakdown until between pole plate writes down its voltage breakdown as the experiment detected value;
(3) the voltage breakdown detected value with step (2) compares with selected standard value; This standard value is measured for through above-mentioned experimental technique the good inorganic nanoparticles compound polyimide film raw material of dispersion of the polyimide raw material that do not add nano particle and standard being carried out standard test; Repeatedly measure and average, with the gained experimental result as standard value;
(4) testing result analysis: detected value and standard value are approaching more, explain that nanoparticulate dispersed is even more in the sample, and inorganic nanoparticles compound polyimide film raw material dispersiveness is good more.
The good Kapton raw material of used dispersion was to confirm that through scanning electron microscopy measurement its dispersiveness is good during said step (3) standard value was confirmed.
Advantage of the present invention and beneficial effect:
1. compare with sedimentation, detection method provided by the present invention need not to wait for the sedimentation of inorganic nanoparticles compound polyimide film raw material, can save time;
2. need not inorganic nanoparticles compound polyimide film raw material is handled (like dilution etc.), can directly detect the dispersiveness of inorganic nanoparticles compound polyimide film raw material, the result is accurate;
3. do not receive the restriction of various stably dispersing mechanism;
4. do not receive the restriction of inorganic nanoparticles compound polyimide film raw material viscosity;
5. it is simple, easy to operate to detect used experimental facilities, and experimental result is directly perceived, accurate.
Description of drawings
Fig. 1 is the used experiment device schematic diagram of the present invention;
Fig. 2 is the dispersed detection method process flow diagram of inorganic nanoparticles compound polyimide film raw material of the present invention.
Reference numeral of the present invention is following:
1---AC power 2---resistance
3---insulation bracing frame 4---lithographic plate electrode
5---detection receptacle 6---specimen
Embodiment
Through specific embodiment the present invention is further described below.
The present invention is based on the shelf depreciation principle,, detect the dispersion stabilization of nano particle in the inorganic nanoparticles compound polyimide film raw material through measuring the voltage breakdown of inorganic nanoparticles compound polyimide film raw material.
Have only regional area to discharge in the insulator, and do not run through between the conductor that applies voltage, this phenomenon is referred to as shelf depreciation.Shelf depreciation among the present invention occurs in the inside of insulator one inorganic nanoparticles compound polyimide film raw material, is inner shelf depreciation.Because inorganic nanoparticles compound polyimide film raw material is made up of compound substance, the electric field intensity in different materials is different, and breakdown field strength is also different, and this just shelf depreciation possibly at first occur in certain material.If nanoparticulate dispersed is inhomogeneous in the inorganic nanoparticles compound polyimide film raw material; Nano particle is reunited; Then the nano particle place of cohesion tends at first take place shelf depreciation, finally causes inorganic nanoparticles compound polyimide film raw material to puncture.
The breakdown voltage value that detects the gained sample is low more, explains that this inorganic nanoparticles compound polyimide film raw material dispersiveness is poor more; The voltage breakdown of detection gained sample is the value of being near the mark more, explains that then this inorganic nanoparticles compound polyimide film raw material dispersiveness is good more.
The present invention utilizes pick-up unit as shown in Figure 1; The upper end of detection receptacle 5 is provided with insulation bracing frame 3, is fixed with two lithographic plate electrodes 4 above the insulation bracing frame 3, has a lithographic plate electrode to be connected with resistance 2; The other end of resistance 2 connects high-voltage ac power, the direct ground connection of another lithographic plate electrode; During test sample is filled detection receptacle 5.
Detection method of the present invention is as shown in Figure 2.
Embodiment 1 (the voltage tester sample settles the standard)
(1) at the nano combined Kapton of prepared in laboratory.Nano particle is handled to improve its dispersiveness through surface conditioning agent in the preparation process, in the nano particle dispersion process, adopts ultrasonic and mechanical blending method, fully the dispersing nanometer particle.Inorganic nano/the polyamic acid solution that makes is divided into two parts; Finished film is processed in the film imidization of a shop; And finished product is passed through the scanning electron microscope imaging confirm its dispersiveness, favorable dispersibility is then got another part inorganic nano/polyamic acid solution as the normal voltage test sample book.
(2) Kapton raw material to be measured is poured in the diagram pick-up unit, container is filled, and go down except that bubble, in this sample, put into the metal plate electrode again in vacuum environment;
(3) press the CC of circuit shown in the synoptic diagram, apply the 0-10kV alternating voltage, press 0.5kV/s speed and increase voltage magnitude to two-plate, the Kapton raw material discharge breakdown until between pole plate, record voltage breakdown this moment is 4.1kV;
(4) repeat above-mentioned steps four times, and to write down breakdown voltage value respectively be 4.0kV, 4.3kV, 4.1kV, 4.2kV.Above-mentioned five mean value results are 4.14kV, with this magnitude of voltage as a standard value.
(1) the nano combined Kapton of prepared in laboratory, nanoparticle surface is untreated in the preparation process, adopts pure mechanical dispersion process that nano particle is disperseed, and the nano combined Kapton raw material that makes is got quantitative as detecting sample.Method is same as embodiment 1, and standard value is the 4.14kV of embodiment 1.
(2) Kapton raw material to be measured is poured in the diagram pick-up unit, container is filled, and go down except that bubble, in this sample, put into the metal plate electrode again in vacuum environment;
(3) press the CC of circuit shown in the synoptic diagram, apply the 0-10kV alternating voltage, press 0.5kV/s speed and increase voltage magnitude to two-plate, the Kapton raw material discharge breakdown until between pole plate, record voltage breakdown this moment is 3.1kV;
(4) the voltage breakdown detected value of step (3) and the standard value 4.14kV of step 1 are compared, find that its breakdown voltage value is lower than standard value, difference assert that greater than 20% this sample dispersiveness is relatively poor.
(1) gets in the actual industrial production process nano combined Kapton raw material as detecting cost.Standard value still is the 4.14kV of embodiment 1.
(2) Kapton raw material to be measured is poured in the diagram pick-up unit, container is filled, and go down except that bubble, in this sample, put into the metal plate electrode again in vacuum environment;
(3) press the CC of circuit shown in the synoptic diagram, apply the 0-10kV alternating voltage, press 0.5kV/s speed and increase voltage magnitude to two-plate, the Kapton raw material discharge breakdown until between pole plate, record voltage breakdown this moment is 4.0kV;
(4) the voltage breakdown detected value of step (3) and the standard value 4.14kV of step 1 are compared, find to approach standard value, difference is assert this sample favorable dispersibility within 5%.
The present invention is mainly in the electric insulation technical field.
Claims (2)
1. the dispersed detection method of an inorganic nanoparticles compound polyimide film raw material has following steps:
(1) gets inorganic nano combined Kapton raw material to be measured and pour in the detection receptacle, container is filled, and go down except that bubble, in this sample, put into the metal plate electrode again in vacuum environment;
(2) apply the 0-10kV alternating voltage to two-plate, begin to increase voltage magnitude by 0.5kV/s speed from 0kV, the inorganic nanoparticles compound polyimide film raw material discharge breakdown until between pole plate writes down its voltage breakdown as the experiment detected value;
(3) the voltage breakdown detected value with step (2) compares with selected standard value; This standard value is measured for through above-mentioned experimental technique the good inorganic nanoparticles compound polyimide film raw material of dispersion of the polyimide raw material that do not add nano particle and standard being carried out standard test; Repeatedly measure and average, with the gained experimental result as standard value;
(4) testing result analysis: detected value and standard value are approaching more, explain that nanoparticulate dispersed is even more in the sample, and inorganic nanoparticles compound polyimide film raw material dispersiveness is good more.
2. the detection method dispersed according to a kind of inorganic nanoparticles compound polyimide film raw material of claim 1; It is characterized in that the good Kapton raw material of used dispersion was to confirm that through scanning electron microscopy measurement its dispersiveness is good during said step (3) standard value was confirmed.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105388053A (en) * | 2015-11-11 | 2016-03-09 | 云南磷化集团有限公司 | Method for processing micro-fine particle sample in flake production process |
| CN107621434A (en) * | 2017-11-03 | 2018-01-23 | 江苏省交通技师学院 | A kind of nanometer diesel oil dispersion stabilization evaluation device |
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| WO2021120516A1 (en) * | 2019-12-19 | 2021-06-24 | 南京中鸿润宁新材料科技有限公司 | Method for detecting corona resistance performance of polyimide composite film material |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004107658A (en) * | 2002-08-28 | 2004-04-08 | Du Pont Toray Co Ltd | Polyimide film and method for producing the same |
| CN101381514A (en) * | 2008-09-11 | 2009-03-11 | 东华大学 | Method for improving dispersion of nano silica granules in polyimide resin |
-
2012
- 2012-01-12 CN CN201210009376XA patent/CN102590047B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004107658A (en) * | 2002-08-28 | 2004-04-08 | Du Pont Toray Co Ltd | Polyimide film and method for producing the same |
| CN101381514A (en) * | 2008-09-11 | 2009-03-11 | 东华大学 | Method for improving dispersion of nano silica granules in polyimide resin |
Non-Patent Citations (2)
| Title |
|---|
| ELI RUCKENSTEIN等: "《nanocomposites of rigid polyamide dispersed in flexible vinyl polymer》", 《POLYMER》 * |
| 李元庆等: "《聚酰亚胺纳米杂化薄膜绝缘材料77k下得电击穿性能研究》", 《第九届全国绝缘材料与绝缘技术学术交流会论文集》 * |
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| CN107621434A (en) * | 2017-11-03 | 2018-01-23 | 江苏省交通技师学院 | A kind of nanometer diesel oil dispersion stabilization evaluation device |
| CN108593737A (en) * | 2018-05-07 | 2018-09-28 | 辽宁科技大学 | Polyimides electrochemical sensing original paper and preparation method thereof and sensor |
| CN109470616A (en) * | 2018-10-31 | 2019-03-15 | 重庆大学 | Rock multifunction seepage test macro |
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| CN109916941B (en) * | 2019-03-25 | 2021-04-30 | 苏州大学 | 3D printing separation detection method for premixed powder |
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| CN113588880A (en) * | 2021-07-28 | 2021-11-02 | 广东九彩新材料有限公司 | Carbon black master batch dispersibility detection equipment and method |
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