CN105842139A - Method for determining percolation threshold of pressure-sensitive microspheres in nonlinear insulation material - Google Patents
Method for determining percolation threshold of pressure-sensitive microspheres in nonlinear insulation material Download PDFInfo
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- 239000004005 microsphere Substances 0.000 title claims abstract description 46
- 238000005325 percolation Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000012774 insulation material Substances 0.000 title abstract 2
- 239000011159 matrix material Substances 0.000 claims abstract description 17
- 238000012360 testing method Methods 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 15
- 239000000945 filler Substances 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000009413 insulation Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000012216 screening Methods 0.000 claims abstract description 7
- 230000004044 response Effects 0.000 claims abstract description 4
- 239000003989 dielectric material Substances 0.000 claims description 14
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- 239000007788 liquid Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 239000004593 Epoxy Substances 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000011810 insulating material Substances 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 230000000704 physical effect Effects 0.000 claims description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
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- 229910052737 gold Inorganic materials 0.000 abstract 1
- 238000007747 plating Methods 0.000 abstract 1
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- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
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- 238000010586 diagram Methods 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Inorganic materials O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
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- 229960000935 dehydrated alcohol Drugs 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- YEAUATLBSVJFOY-UHFFFAOYSA-N tetraantimony hexaoxide Chemical compound O1[Sb](O2)O[Sb]3O[Sb]1O[Sb]2O3 YEAUATLBSVJFOY-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0272—Investigating particle size or size distribution with screening; with classification by filtering
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Abstract
The invention relates to a method for determining the percolation threshold of pressure-sensitive microspheres in a nonlinear insulation material. The method comprises the following steps: 1, preparing a nonlinear composite sample: 1) screening the pressure-sensitive microspheres, and 2) mixing materials; and 2, testing the volt-ampere characteristic of a nonlinear compound: carrying out direct current volt-ampere characteristic test on the above obtained nonlinear compound forming an electrode through a gold plating technology, continuously improving the test voltage, measuring the response current flowing through the sample, and obtaining the J(E) characteristic of the compound sample according to the formula (1) involving the measured voltage (U) and the current (I): J = I/S and E = U/d. The standardized method for determining the percolation threshold of the compound is provided to solve the problem of change of the percolation threshold of the nonlinear compound with the characteristics of a matrix of a pressure-sensitive microsphere filler, so characteristic parameters are provided for the preparation of the nonlinear compound and an application of the nonlinear compound in high voltage insulation devices.
Description
Technical field
The present invention relates to the testing research technical field of electrical material field Nonlinear Composite, be specially really
The method of the percolation threshold of pressure-sensitive microsphere in determining non-linear dielectric materials.
Background technology
Insulator arrangement in alternating current-direct current power transmission and transformation system or parts, the Electric Field Distribution himself born often pole
Uneven, the insulated part of such as power cable termination, the high-pressure side part of various insulator, sleeve pipe etc.,
The electric field intensity born will be far beyond the meansigma methods of overall electric field intensity, the even up to several times of meansigma methods,
Thus bring the adverse effect of a series of design, manufacture view.Further, since insulator arrangement or parts are certainly
Body bears the inhomogeneities of Electric Field Distribution, and electric field intensity is relatively big, especially causes corona, shelf depreciation occur
Etc. the dielectric substance at the position of phenomenon, its aging speed the most faster, degree even more serious, the most right
The long-term safety stable operation of system brings bigger threat.Therefore, rationally improve insulator arrangement or parts are whole
Bulk electric field distribution uniformity coefficient, relax local high electric field intensity, can reduce extra-high voltage equipment design,
The technical difficulty manufactured, reduces power equipment cost, is greatly saved power construction investment, and it is long to improve equipment
The security reliability that phase is run.Compared with the traditional method using various the exterior measures, by various different materials
Material regulates the performance parameter of insulative dielectric material self, it is achieved improve insulator arrangement or parts Electric Field Distribution
The effect of uniformity coefficient, is the method widely used at present, all presses effect in reality, and reduction equipment sets
The aspects such as meter, manufacture difficulty, all have obvious advantage.In all kinds of insulant, there is high level non-
The insulant of linear electrology characteristic can reach the most in terms of the distortion of suppression internal field, uniform field strength distribution
Preferably effect, has a wide range of applications.
According to correlational study, fill a certain amount of in the organic polymer insulant such as epoxy resin, silicone rubber
The new blend that generated of miniature varistor granule can show the Gao Shui similar with based varistor
Flat non-linear electric character, be applied to electric field in insulator arrangement be susceptible to distortion key position can body
Reveal following advantage: there is higher insulation resistance value, and under higher electric field intensity, carry out mild tune
Joint, can bear continuous print operation voltage, still keep relatively low power consumption under ac high voltage, have good
Thermal conduction characteristic;At transient characterisitics fast response time, regulatable non-linear domain is gathered than traditional gradient fields
Close high two orders of magnitude of insulant, can be widely used in the insulation of electrical installation including cable, sleeve pipe etc.
Electric field regulation and control in.
Current miniature varistor granule in non-linear complex as filler is mainly spherical ZnO pressure
Quick pottery (the lower abbreviation pressure-sensitive microsphere of ZnO), and the actual selection applied for packing volume mark has more
Harsh requirement.First, the volume fraction of filler has lower limit, because only that when ZnO pressure-sensitive microsphere filler
Complex ability when volume fraction exceedes the percolation threshold of such " filler/polymeric matrix " this dispersion
Enough show stable non-linear electric character.And more than percolation threshold, the volume fraction of filler is the lowest
The best, because filler is dropped for the impact of other physical characteristics of insulant such as thermal characteristics, mechanical property
To minimum.Therefore, packing volume mark is to be advisable just above percolation threshold, it means that have in preparation
Before the composite of non-linear electric character, need first to determine the percolation threshold of such complex.Although it is reasonable
The percolation threshold of the opinion research report its theory of complex with spheroidal particle as filler as 16%vol about, but real
On border, the percolation threshold of complex is affected greatly by the microstructure of filler and polymeric matrix, typically
The shape of influence factor's such as filler, particle diameter, or the elastic modelling quantity of matrix and pyrocondensation characteristic etc..Therefore, by reality
The percolation threshold of each quasi-nonlinear complex that test obtains is between 15%vol to 40%vol, and current
Most scholars think that ZnO complex to show its packing volume mark of stable non-linear electric character and need
Will be at more than 40%vol.Therefore, application is put at every kind of non-linear complex with pressure-sensitive microsphere as filler
Before, need first to measure the percolation threshold of this insulation system.
Summary of the invention
It is an object of the invention to provide the side of the percolation threshold of pressure-sensitive microsphere in determining non-linear dielectric materials
Method, with the problem solving to propose in above-mentioned background technology.
For achieving the above object, the present invention provides following technical scheme: pressure-sensitive in determining non-linear dielectric materials
The method of the percolation threshold of microsphere, comprises the following steps:
Prepared by S1, non-linear composite sample:
S11, the screening of pressure-sensitive microsphere: the pressure-sensitive microsphere prepared is screened, packing material size is controlled
In certain limit, and depending on this scope also will be according to the overall particle diameter distribution of microsphere;
S12, batch mixing: pressure-sensitive microsphere mixes with organic insulation polymeric matrix according to different volumes mark;
S2, the test of non-linear complex C-V characteristic: to the non-linear complex prepared according to the method described above
The C-V characteristic carried out under direct current after gold-plated method is by electrode is tested, and i.e. improves constantly test voltage, measures stream
Cross the response current of sample;Complex sample can be obtained by formula (1) by the voltage (U) recorded and electric current (I)
J (E) characteristic of product, J=I/S, E=U/d, wherein J is electric current density, and E is the field intensity being applied on sample,
S is that example cross section amasss, and d is thickness of sample, J (E) characteristic obtained.
In step S11, the particle diameter of described pressure-sensitive microsphere is distributed in the particle diameter between 50-150 μm, after screening
Difference is in 25 μm.
In step S12, depending on mixing method is according to the physical property of insulating material matrix.
For the epoxy resin-base become solid when heated for liquid under room temperature, by microsphere with epoxy resin at beaker
Middle stirring, carries out vacuum and pours and be heating and curing molding after being sufficiently mixed.
For being solid under room temperature, but more liquid matrix, by matrix with pressure-sensitive microsphere filler large-scale
In high torque (HT) agitator stirring mixing, or be dissolved in solution stirring mix solvent evaporated again, finally
Mixture is heated in tablet machine extrusion forming.
For under room temperature be solid-state and hardness the highest, and be insoluble in the matrix of organic solvent, at instrumentation
Inside carry out melt blending, then carry out the compression molding operation of pressurized, heated.
In step S2, volume fraction composite sample below percolation threshold shows and common insulant
Similar close to linear C-V characteristic.
In step S2, it is special that volume fraction composite sample more than percolation threshold can show non-linear volt-ampere
Property, and its breakdown voltage gradient reduces along with the increase of composite body fraction.
In step S2, volume fraction composite sample near percolation threshold gets final product body at lower voltages
Reveal breakdown characteristics, and after sample shows breakdown characteristics in testing, the most anti-to same sample again
Carry out C-V characteristic test again, then sample presents the nonlinear wind vibration of standard in follow-up test, thus
The volume fraction of this complex is considered as in corresponding particle size range " filler-polymeric matrix " this insulation system
Percolation threshold.
Compared with prior art, the invention has the beneficial effects as follows: it is contemplated that for non-linear complex
The problem that percolation threshold changes such as matrix or pressure-sensitive microsphere packing property, proposes one and measures multiple
The normalized method of compound percolation threshold, thus for the preparation of non-linear complex and set in High-Voltage Insulation
Standby upper Application Design provides characteristic parameter.
Accompanying drawing explanation
Fig. 1 is volume fraction pressure-sensitive microsphere distribution signal in the non-linear complex that percolation threshold is higher above
Figure;
Fig. 2 is pressure-sensitive microsphere distribution signal in the non-linear complex that volume fraction is slightly higher more than percolation threshold
Figure
Fig. 3 is pressure-sensitive microsphere distribution schematic diagram in the volume fraction non-linear complex near percolation threshold
Fig. 4 is pressure-sensitive microsphere distribution schematic diagram in the volume fraction non-linear complex below percolation threshold
Fig. 5 is that J (E) characteristic of the non-linear complex of the pressure-sensitive microsphere/silicone rubber of ZnO under different volumes mark is bent
Line;
Fig. 6 is J (E) characteristic curve that the follow-up measurement after 35%vol sample is measured first and punctured obtains.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clearly
Chu, be fully described by, it is clear that described embodiment be only a part of embodiment of the present invention rather than
Whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creation
The every other embodiment obtained under property work premise, broadly falls into the scope of protection of the invention.
1-accompanying drawing 4 referring to the drawings, according in the non-linear complex of measurement of patent specification introduction of the present invention
The method of pressure-sensitive microsphere percolation threshold, the actual ZnO/ silicone rubber non-thread measured with the pressure-sensitive microsphere of ZnO as filler
The percolation threshold of property complex:
(1) prepared by non-linear composite sample:
1) preparation of pressure-sensitive microsphere and screening
Various metal-oxides in formula are mixed in following ratio: 95mol%ZnO+1.0mol%
Bi2O3+ 0.5mol%MnO2+ 1.0mol%Co2O3+ 0.4mol%Cr2O3+ 1mol%Sb2O3+1.0
Mol%SiO2And 0.1mol%Al2O3.Again with dehydrated alcohol as ball-milling medium, the powder prepared is put into
Planetary ball mill mixes 8 hours.Then divided addition organic bond to be placed on spraying to make by be arranged to
Carry out mist projection granulating after grain drying machine, obtain spherical binding.Hereafter the product obtained is sieved, then with
The programming rate of 0.55 DEG C/min rises to 1200 DEG C and sinters 4.5 hours, is cooled to the speed of 16 DEG C/min
Room temperature, is finally scattered in screening to product, obtains micro-in 60-80 μm particle size range of particle size range
Type ZnO varistor (pressure-sensitive microsphere).
2) batch mixing
Above-mentioned for ZnO prepared ZnO pressure-sensitive microsphere uniform filling is scattered in silicon rubber by li quid mixing method by experiment
In glue, process is as follows: double two or five vulcanizing agents that 110 silicone rubber and mass ratio are 0.8% are dissolved in a small amount of four
In hydrogen THF solvent, after using the mechanical agitator stir about 20min that torque is bigger, silicone rubber is complete with vulcanizing agent
CL in solvent, then will according to volume fraction (25%vol, 31%vol, 35%vol, 39%vol, 43%vol,
47%vol) calculate load weighted pressure-sensitive microsphere filler powder body to be placed in mixed system, continue stirring 2-3 hour
So that major part solvent volatilization.Mixed raw material is put into baking oven, 60 DEG C of freeze-day with constant temperature, thing table to be mixed
After face no longer produces bubble, then dry one hour, make the oxolane of inside volatilize completely.Gained is mixed
Compound also needs further compression molding: put in vulcanizer by the mixture of about 3g, at 15MPA every time
Being cooled to room temperature after hot pressing 15min at a temperature of pressure and 170 DEG C, obtaining thickness, to be about 0.5mm a diameter of
The round shape thin slice of 20mm.
(2) test of non-linear complex C-V characteristic
For the non-linear complex prepared according to the method described above, at each print upper and lower surface gold-plated electrode
Recorded the C-V characteristic of each print afterwards by keithley2410C data multimeter and data collecting system, survey
The ladder incremental voltage of pilot production 1-1100V, totally 1101 voltage sample points, current limit is 0.1mA.
J (E) characteristic of composite sample can be obtained by formula (1) by the voltage (U) recorded and electric current (I),
J=I/S
(1)
E=U/d
Wherein J is electric current density, and E is the field intensity being applied on sample, and S is that example cross section amasss, and d is sample
Product thickness.
As shown in Figure 5, wherein 31%vol, 25%vol sample embodies J (E) characteristic obtained the most in testing
Go out nonlinear characteristic, embody the most in the drawings;And 39%vol, 43%vol, 47%vol sample embodies
The nonlinear wind vibration of standard;35%vol sample shows breakdown characteristics, after it shows breakdown characteristics
Immediately to its C-V characteristic of same sample repeated measurement, obtain J (E) curve as shown in Figure 6, it is seen that its
Follow-up measurement also present typical nonlinear characteristic, thus may determine that packing material size is in 60-80 μm
The pressure-sensitive microsphere of ZnO/silicone rubber compound percolation threshold be about 35%vol.
Although the present invention being described in detail with reference to previous embodiment, for those skilled in the art
For, the technical scheme described in foregoing embodiments still can be modified by it, or in the middle part of it
Point technical characteristic carries out equivalent, all within the spirit and principles in the present invention, any amendment of being made,
Equivalent, improvement etc., should be included within the scope of the present invention.
Claims (9)
1. the method for the percolation threshold of pressure-sensitive microsphere in determining non-linear dielectric materials, it is characterised in that: include
Following steps:
Prepared by S1, non-linear composite sample:
S11, the screening of pressure-sensitive microsphere: the pressure-sensitive microsphere prepared is screened, packing material size is controlled
In certain limit, and depending on this scope also will be according to the overall particle diameter distribution of microsphere;
S12, batch mixing: pressure-sensitive microsphere mixes with organic insulation polymeric matrix according to different volumes mark;
S2, the test of non-linear complex C-V characteristic: to the non-linear complex prepared according to the method described above
The C-V characteristic carried out under direct current after gold-plated method is by electrode is tested, and i.e. improves constantly test voltage, measures stream
Cross the response current of sample;Complex sample can be obtained by formula (1) by the voltage (U) recorded and electric current (I)
J (E) characteristic of product, J=I/S, E=U/d, wherein J is electric current density, and E is the field intensity being applied on sample,
S is that example cross section amasss, and d is thickness of sample, J (E) characteristic obtained.
The most according to claim 1 determine non-linear dielectric materials in the side of percolation threshold of pressure-sensitive microsphere
Method, it is characterised in that: in step S11, the particle diameter of described pressure-sensitive microsphere is distributed between 50-150 μm,
Particle diameter difference after screening is in 25 μm.
The most according to claim 1 determine non-linear dielectric materials in the side of percolation threshold of pressure-sensitive microsphere
Method, it is characterised in that: in step S12, depending on mixing method is according to the physical property of insulating material matrix.
The most according to claim 3 determine non-linear dielectric materials in the side of percolation threshold of pressure-sensitive microsphere
Method, it is characterised in that: for the epoxy resin-base become solid when heated for liquid under room temperature, by microsphere and ring
Epoxy resins stirs in beaker, carries out vacuum and pour and be heating and curing molding after being sufficiently mixed.
The most according to claim 3 determine non-linear dielectric materials in the side of percolation threshold of pressure-sensitive microsphere
Method, it is characterised in that: for being solid under room temperature, but more liquid matrix, matrix is micro-with pressure-sensitive
Ball filler stirs mixing in large-scale high torque (HT) agitator, or is dissolved in solution stirring mixing and steams
Dry solvent, finally heats extrusion forming in tablet machine by mixture.
The most according to claim 3 determine non-linear dielectric materials in the side of percolation threshold of pressure-sensitive microsphere
Method, it is characterised in that: under room temperature be solid-state and hardness the highest, and be insoluble in the matrix of organic solvent,
In instrumentation, carry out melt blending, then carry out the compression molding operation of pressurized, heated.
The most according to claim 1 determine non-linear dielectric materials in the side of percolation threshold of pressure-sensitive microsphere
Method, it is characterised in that: in step S2, volume fraction composite sample below percolation threshold show with
Common insulant similar close to linear C-V characteristic.
The most according to claim 1 determine non-linear dielectric materials in the side of percolation threshold of pressure-sensitive microsphere
Method, it is characterised in that: in step S2, volume fraction composite sample more than percolation threshold can show
Nonlinear wind vibration, and its breakdown voltage gradient reduces along with the increase of composite body fraction.
The most according to claim 1 determine non-linear dielectric materials in the side of percolation threshold of pressure-sensitive microsphere
Method, it is characterised in that: in step S2, volume fraction composite sample near percolation threshold is relatively low
Breakdown characteristics is i.e. reflected under voltage, and after sample shows breakdown characteristics in testing, the most again
Same sample is repeated C-V characteristic test, then sample presents the non-linear volt of standard in follow-up test
Peace characteristic, is thus considered as the volume fraction of this complex in corresponding particle size range " filler-polymeric matrix "
The percolation threshold of this insulation system.
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Cited By (6)
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RU2650987C2 (en) * | 2016-10-05 | 2018-04-18 | Российская Федерация, от имени которой выступает Государственная корпорация по атомной энергии "Росатом" (Госкорпорация "Росатом") | Microspheres selection method by strength to set pressure |
CN111875965A (en) * | 2020-07-17 | 2020-11-03 | 清华大学 | Electric field self-adaptive composite material based on surface functionalization treatment and preparation method thereof |
CN111909518A (en) * | 2020-07-24 | 2020-11-10 | 清华大学 | Preparation method of composite material taking high-temperature vulcanized solid silicon rubber as matrix |
CN111961313A (en) * | 2020-07-23 | 2020-11-20 | 清华大学 | Self-adaptive electric field regulation and control composite material based on gradient distribution and preparation method thereof |
CN111978730A (en) * | 2020-07-17 | 2020-11-24 | 清华大学 | Electric field self-adaptive composite material based on particle size combination and preparation method thereof |
CN114486896A (en) * | 2022-01-30 | 2022-05-13 | 浙江大学 | Equipment and method capable of monitoring melting and seepage characteristics of sintering liquid phase on line |
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