CN109627049A - A method of improving energy storage ceramic material dielectric constant - Google Patents
A method of improving energy storage ceramic material dielectric constant Download PDFInfo
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- CN109627049A CN109627049A CN201710929846.7A CN201710929846A CN109627049A CN 109627049 A CN109627049 A CN 109627049A CN 201710929846 A CN201710929846 A CN 201710929846A CN 109627049 A CN109627049 A CN 109627049A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
- C04B41/5116—Ag or Au
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/88—Metals
Abstract
The invention discloses a kind of methods for improving energy storage ceramic material dielectric constant, technology for preparing electrode is adjusted by using following methods, (1) silver paste is improved in the solidification temperature on ceramics sample surface, with the raising of silver ink firing temperature, dielectric constant greatly improves, and dielectric properties are best at 880 DEG C；(2) extend soaking time at a temperature of 880 DEG C of silver ink firings, be optimal dielectric properties in 3h or so；(3) it is simulated by Zview software, and announcement will show superior dielectric properties in wider higher frequency and must reduce sheet resistance.Method provided by the invention is not only able to improve the performances such as the dielectric constant of energy storage ceramic material, also theoretically analyzes the implementation method for and guiding such dielectric material to play superior dielectric properties.
Description
Technical field
The present invention relates to technical field of function materials, more particularly to a kind of raising energy storage ceramic dielectric material is normal
Several methods.
Background technique
Strontium titanates (SrTiO3) ceramics are a kind of important functional materials, it is widely used in the fields such as electronics, mechanical industry.
Strontium titanate ceramics are cube phase structure at room temperature, are paraelectrics, relative dielectric constant with higher, and since it is unlike iron
Electric body ceramics (such as BaTiO3) internal like that there are the unstable of domain wall, therefore strontium titanate ceramics proof voltage also with higher is strong
Degree, to be provided simultaneously with the peculiar property of higher ε r and Eb.Thus in recent years, strontium titanate ceramic is considered as that great development is latent
One of solid-state energy-accumulating medium material system of power.
It can be seen that realizing that the key of more high energy storage density is to obtain higher opposite dielectric simultaneously in strontium titanate ceramics
Constant and dieletric strength.However, since the relative dielectric constant and dieletric strength of dielectric material are a pair of conflicting
Parameter.Therefore, the research of strontium titanate ceramic energy storage material never has the progress of making a breakthrough property, in order to improve Jie of material
Electric constant and breakdown strength, researcher use a variety of methods such as doping, additive, cladding.Such as by Ba2+Substitute Sr2+Position, though
It so improves dielectric constant but is reduction of breakdown strength, so that energy storage density does not have raising；Low-k addition is added
Agent, although can reduce crystallite dimension improves breakdown strength, dielectric constant decline is violent.Therefore, improve dielectric material performance
Method it is different, superiority and inferiority is also different.And most important problem is, these improve the essence of material property method, i.e. physical model
It is not very clearly that this, which results in largely testing, attempts still cannot finally meet the needs of optimal performance material.
Summary of the invention
The capacity measurement of usual dielectric ceramic material needs to coat electrocondution slurry on the two sides of sheet sample, is formed after solidification
Bipolar plates.But whether electric conductivity, the electric conductivity of sample surfaces and electrode contact well simultaneously with sample after electrode material solidifies
Without deeper discussion, and this point plays superior dielectric properties to dielectric material and has a major impact.
In view of this, not only improving metatitanic acid the present invention provides a kind of method for improving energy storage ceramic material dielectric constant
The performances such as the dielectric constant of strontium dielectric material, also theoretically analysis and guides such dielectric material to play superior dielectric properties
Implementation method.
To achieve the goals above, the present invention adopts the following technical scheme:
A method of energy storage ceramic material dielectric constant is improved, includes the following:
(1) silver electrode solidification temperature is improved
By the way that silver paste is uniformly applied on strontium titanate ceramics sample using oil painting brush, it is to be dried after by the strontium titanates
Ceramics sample, which is put into batch-type furnace, to be solidified, and chooses 580 DEG C, 680 DEG C, 780 DEG C and 880 DEG C of solidification temperature, soaking time is equal
For 30~35min, the dielectric constant under the corresponding dielectric and magnetic of silver electrode solidification temperature and high frequency is measured, then to obtain most
Good solidification temperature, as shown in Figure 2.
(2) extend electrode curing time
Silver paste is evenly coated in strontium titanates sample surfaces, it is 880 DEG C of conditions that best curing temperature is chosen in batch-type furnace
Under, it selects 0.5,1,1.5,2,2.5,3,3.5 and 4h to be heating and curing sample silver electrode respectively, it is solid then to measure silver electrode
Change the dielectric constant under time corresponding dielectric and magnetic and high frequency, it is best solid under the conditions of optimal solidification temperature to obtain
Change the time, as shown in Figure 3.
(3) Zview software is simulated
The model of selection is two RC parallel units series connection, and parameter is C1=10nF, C2=100nF, R2=10M respectively
Ω, R1 value are 1000,100,10,1,0.1,0.01 and 0.001 Ω, then varying with frequency to the capacitor of system and loss
Relational graph is simulated, to carry out analogy with the data of actual experiment, as shown in Figure 5,6.
It can be seen via above technical scheme that compared with prior art, the present disclosure provides a kind of raising energy storage potteries
The method of ceramic material dielectric constant is adjusted technology for preparing electrode by using following methods, and (1) improves silver paste and making pottery
The solidification temperature of porcelain sample surfaces, with the raising of silver ink firing temperature, dielectric constant is greatly improved, and dielectric properties are best at 880 DEG C；
(2) extend soaking time at a temperature of 880 DEG C of silver ink firings, be optimal dielectric properties in 3h or so；(3) pass through Zview software mould
It is quasi-, and announcement will show superior dielectric properties in wider higher frequency and must reduce sheet resistance.
In addition, the example for improving material dielectric constant in the past generally lays particular emphasis on the research of material nature, and this patent
It is used as device detection entirety for strontium titanates dielectric material, stresses surface electrode contact part, as shown in figure 4, not only from experiment
In provide practical method, and theoretically simulation propose guidance method, this has the application and performance test of dielectric material
Great importance.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 attached drawing is the block schematic illustration of the method for the present invention.
Fig. 2 attached drawing is to be situated between under the corresponding dielectric and magnetic of strontium titanates polycrystalline ceramics of the present invention change silver ink firing electrode temperature and high frequency
Electric constant is with silver ink firing temperature variation.
Fig. 3 attached drawing is to be situated between under strontium titanates polycrystalline ceramics of the present invention change electrode silver ink firing time corresponding dielectric and magnetic and high frequency
Electric constant is with silver ink firing temperature variation.
Fig. 4 attached drawing is the scanning electron microscope enlarged drawing of different temperatures silver ink firing of the present invention corresponding electrode and sample contact interface.
Fig. 5 attached drawing is the series model figure that Zview of the present invention simulates two RC parallel units.
Fig. 6 attached drawing is the dielectric and magnetic of change R1 resistance value in the series model of two RC parallel units of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In order to improve contact quality of the electrode with sample, the embodiment of the invention discloses a kind of raising energy storage ceramic material Jie
The method of electric constant, to be adjusted to technology for preparing electrode.
A method of energy storage ceramic material dielectric constant is improved, includes the following:
(1) silver electrode solidification temperature is improved:
Silver paste is uniformly applied to the sample one side made with oil painting brush, is placed it in dry in 60 DEG C of drying box
20min also uniformly smears another side after taking-up, is then placed in batch-type furnace (KSL-1100X of Hefei section crystalline substance manufacture) with 4
DEG C/heating rate of min rises to required temperature, and keeps the temperature 30min at desired temperatures.Silver paste is consolidated under normal conditions
Changing temperature is 540 DEG C~590 DEG C, and silver point is about 962 DEG C.To make the brighter of the characteristic performance of silver paste at different temperatures
Aobvious, the present invention chooses 580 DEG C, 680 DEG C, 780 DEG C and 880 DEG C of solidification temperature, finally uses the electrochemistry of Japan HIOKI (IM3590)
Impedance spectrometer measures the dielectric constant under the corresponding dielectric and magnetic of silver electrode solidification temperature and high frequency.
As a result referring to attached drawing 2, attached drawing 2 is that strontium titanates polycrystalline ceramics changes the corresponding dielectric and magnetic (a) of silver ink firing electrode temperature
With dielectric constant (b) under high frequency with silver ink firing temperature variation.It is obtained by formula C=ε s/4k π d, dielectric constant formula is ε=4k π
D/cs, wherein k=9 × 109N is electrostatic force constant, can obtain the spectrogram as shown in figure (a).It is learnt by scheming (b), with silver ink firing
The raising of temperature, dielectric constant also greatly improve, and under same frequency, dielectric constant occurs significantly increasing as the temperature rises
Greatly, the incrementss nearly 1/3 of the dielectric constant from 580 DEG C to 880 DEG C, and advance the speed and tend towards stability, for its performance,
Dielectric properties are best at 880 DEG C.
In addition, result, referring to attached drawing 4, attached drawing 4 is the corresponding electrode of different solidification temperature silver ink firings and sample contact interface
Scanning electron microscope enlarged drawing.Wherein 580 DEG C and 680 DEG C of lower part and 780 DEG C and 880 DEG C of top graininess are electrode layer.By
Figure is learnt, with the raising of solidification temperature, silver electrode layer is finer and close, and the contact with sample surfaces is also closer.
(2) extend electrode curing time:
Strontium titanate ceramics samples one side is uniformly smeared into silver paste, is placed in 60 DEG C of baking oven and toasts 20min, after taking-up
Another side equally uniformly smears silver paste, is held after the completion of smearing with corundum crucible, and is put into batch-type furnace with 4 DEG C/min liter
Temperature, determine silver electrode best curing temperature be 880 DEG C in the case where keep the temperature different time, respectively select 0.5,1,1.5,2,
2.5, sample silver electrode was solidified in 3,3.5 and 4 hours, then measures silver electrode curing time pair with electrochemical impedance spectrometer
Dielectric constant under the dielectric and magnetic and high frequency answered, to obtain the optimum curing time under best curing temperature.
As a result referring to attached drawing 3, attached drawing 3 is that strontium titanates polycrystalline ceramics changes electrode silver ink firing time corresponding dielectric and magnetic (a)
With dielectric constant (b) under high frequency with silver ink firing temperature variation.It is obtained by formula C=ε s/4k π d, dielectric constant formula is ε=4k π
D/cs, wherein k=9 × 109N is electrostatic force constant, can obtain the spectrogram as shown in figure (a).It is learnt by scheming (b), in same temperature
Under degree, declines and tend towards stability in high-frequency region as the increase dielectric constant of frequency is presented, this is because strontium titanate ceramics sample
The property of product itself determines；Under same frequency, with the extension of electrode curing time, dielectric constant is greatly improved,
3.5h reaches maximum, this be for different silver pastes, corresponding to temperature value and the solidification reached under optimum physical characteristic
Time is different, and 880 DEG C, 3.5h layer silver paste some be embedded in ceramics sample surface, contact between the two
Closely, and its contact resistance reaches minimum value, therefore has optimum dielectric properties in 3.5h.
(3) Zview software is simulated:
The model of selection is two RC parallel units series connection, and parameter is C1=10nF, C2=100nF, R2=10M respectively
Ω, R1 value are 1000,100,10,1,0.1,0.01 and 0.001 Ω, then varying with frequency to the capacitor of system and loss
Relational graph is simulated.
As a result referring to attached drawing 5 and attached drawing 6, attached drawing 5 is that Zview simulates two RC parallel units series model figures, model
As a result referring to Fig. 6 (Fig. 6 is the dielectric and magnetic for changing R1 resistance value in the series model of two RC parallel units), by the way that ceramics are situated between
Electrical testing is regarded as to be made of surface and body two parts, and is simulated respectively with a RC parallel units, by changing surface RC
The resistance of unit.
Pass through Fig. 6, it is known that as R1=1k Ω, capacitor occurs as soon as relaxation decline process near 1kHz, with frequency liter
It is high that small capacitances level, and the reduction step by step with R1 from 1000 Ω to 0.01 Ω, the decaying of capacitor are dropped to by bulky capacitor quickly
Process is translated to high frequency, to show the performance of larger capacitance in broader frequency domain.
Know therefrom, as sheet resistance must be reduced if wider higher frequency shows superior dielectric properties, in reality
In example, exactly on the basis of not reducing dielectric material body dielectric properties, sheet resistance is reduced to the greatest extent.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other
The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment
For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part
It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (2)
1. a kind of method for improving energy storage ceramic material dielectric constant, which is characterized in that include the following:
(1) silver electrode solidification temperature is improved
The ingredient of binder in usual slurry includes that synthetic resin has epoxy resin, alkyd resin, acrylic resin, polyurethane
Resin, melamine resin, phenolic resin, vinyl chloride-vinyl acetate copolymer resin, and dispersion is added as needed
Agent, slipping agent, coupling agent；Slurry just obtains excellent electrical and physical characteristic in 120 DEG C or more baking 30min, can provide
Good bending, adhesion, hardness and impedance value；By the way that silver paste to be uniformly applied to strontium titanate ceramics sample using oil painting brush
On product, the strontium titanate ceramics sample is put into batch-type furnace after to be dried and is solidified, constant temperature keeps 30~35min, to remove
The organic resin in slurry is removed, using under the corresponding dielectric and magnetic of electrochemical impedance spectrometer measurement silver electrode solidification temperature and high frequency
Dielectric constant；
(2) extend electrode curing time
Silver paste is evenly coated in strontium titanate ceramics sample surfaces, it is 880 DEG C of conditions that solidification optimum temperature is chosen in batch-type furnace
Under, it selects 0.5,1,1.5,2,2.5,3,3.5 and 4h to solidify sample silver electrode respectively, then uses electrochemical impedance spectrometer
Measure the dielectric constant under silver electrode curing time corresponding dielectric and magnetic and high frequency；
(3) Zview software is simulated
The model of selection is two RC parallel units series connection, by fixed wherein certain the several parameter of control variate method, for example is fixed
C1=10nF, C2=100nF, R2=10M Ω, R1 value are 1000,100,10,1,0.1,0.01 and 0.001 Ω, i.e., by changing
Become different R and C to simulate the capacitor for the system of probing into and relationship varying with frequency is lost, so as to the number with sample actual conditions
According to being compared.
2. in a kind of method for improving energy storage ceramic material dielectric constant according to claim 1, the solidification temperature packet
Include 580 DEG C, 680 DEG C, 780 DEG C or 880 DEG C.
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Application publication date: 20190416 |