CN103021653B - A kind of non-plumbum ferroelectric thick film and preparation method mixing glass dust high energy storage density - Google Patents
A kind of non-plumbum ferroelectric thick film and preparation method mixing glass dust high energy storage density Download PDFInfo
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Abstract
The invention belongs to electronic material and device arts, relate to a kind of non-plumbum ferroelectric thick-film material with high energy storage density.The present invention includes following chemical constituent: in mass ratio: (Na
0.5* ( 1+x )bi
0.5* (1+y)) TiO
3: glass dust: binding agent=1:0.05 ~ 0.3:0.3 ~ 0.6, wherein: 0≤x≤0.05,0≤y≤0.1.Non-plumbum ferroelectric thick film in the present invention solves the environmental pollution that leadwork in use causes, and by doped-glass powder, energy storage density is improved further, can be used as the critical component of high-power high-capacity capacitor development and application.
Description
Technical field
The invention belongs to electronic material and device arts, relate to a kind of there is the non-plumbum ferroelectric thick-film material of high energy storage density preparation and glass dust adulterate and optimize, be applicable to the development and application of high-power high-capacity holding capacitor.
Background technology
In the last few years, along with the rapid growth of industry-by-industry for microelectric technique demand, microelectronic industry was developed rapidly.But microelectronic component moves towards one of microminiaturized, integrated key technology is prepare high-power high-capacity capacitor.Prepare high-power high-capacity capacitor and then require that dielectric substance can deposit electricity fast while having high energy storage density.High energy storage density requires that dielectric substance has high disruptive field intensity and larger polarization value, and traditional ferroelectric block materials, because required operating voltage is higher and disruptive field intensity is less, limits its application; And though thin-film material has higher disruptive field intensity, due to the restriction of thickness, make overall energy storage lower.So ferroelectric thick film material becomes the important channel addressed this problem.
Maximum high-power high-capacity capacitors is used to be all be dielectric capacitor with lead-containing materials substantially in the market.As everyone knows, lead element can produce harm to human body and cause serious pollution to environment in production, use, waste recovery process.The consistent of height has been reached to unleaded in countries in the world.No matter be that leaded dielectric substance is (as PZT; PLZT etc.), or unleaded dielectric substance (as BNT, KNN etc.); the energy storage density of its pure component is all difficult to the level reached needed for reality, usually can improve its performance of optimization by adulterating or adding sintering aid.Glass dust, as a kind of conventional sintering aid, is improving material microstructure, is realizing low-temp liquid-phase sintering, and improving the aspects such as material density has important effect.Thus, the non-plumbum ferroelectric thick-film material that glass dust adds will play an important role in prepared by high-power high-capacity capacitor.
Summary of the invention
The object of the invention is to provide a kind of high-compactness, and the preparation of the non-plumbum ferroelectric thick film of high breakdown field strength and high polarization intensity and glass dust doping optimization method, obtained thick-film material can be used for high-power high-capacity holding capacitor.
Technical scheme of the present invention:
The present invention includes following chemical constituent, in mass ratio, (Na
0.5*(1+x)bi
0.5* (1+y)) TiO
3: glass dust: binding agent=1:0.05 ~ 0.3:0.3 ~ 0.6, wherein: 0≤x≤0.05,0≤y≤0.1.
Described glass dust is with BaCO
3, HBO
3, SiO
2for raw material, BaO:B in molar ratio
2o
3: SiO
2the mixture of=3.5 ~ 5.5:2 ~ 6:0.5 ~ 2.5.
A preparation method for the non-plumbum ferroelectric thick film of the high energy storage density of doped-glass powder, comprises the steps, wherein step 3) and 4) sequentially commutative:
1) powder preparation
Adopt solid reaction process synthesis (Na
0.5*(1+x)bi
0.5* (1+y)) TiO
3powder, wherein: 0≤x≤0.05,0≤y≤0.1, is warming up to 800 ~ 900 DEG C with 3 ~ 10 DEG C/min, is incubated 2 ~ 5 hours, and after cooling with stove, ball milling 5 ~ 10 hours, crosses 300 mesh sieves for subsequent use;
2) glass dust preparation
With BaCO
3, HBO
3, SiO
2for raw material, in molar ratio, BaO:B
2o
3: SiO
2=3.5 ~ 5.5:2 ~ 6:0.5 ~ 2.5 mix, and be warming up to 1000 ~ 1300 DEG C, be incubated 0.5 ~ 3 hour, shrend with 3 ~ 10 DEG C/min, cross 300 mesh sieves for subsequent use;
3) hearth electrode preparation
Adopt silk screen print method on alumina substrate, prepare Ag-Pd electrode;
4) slurry preparation
By 1) powder and 2 prepared of step) glass dust prepared of step, in mass ratio, (Na
0.5*(1+x)bi
0.5* (1+y)) TiO
3powder: glass dust: binding agent=1:0.05 ~ 0.3:0.3 ~ 0.6 is prepared, ground and mixed is obtained thick film ink evenly;
5) thick film preparation
A. by 4) the obtained thick film ink of step adopts silk screen print method to be printed on 3) on Ag-Pd electrode obtained in step, obtain thick film green compact;
B. thick film green compact obtained for a step are got rid of binding agent in 5 hours 550 DEG C of insulations, within 3 ~ 13 hours, sinter 800 ~ 950 DEG C of insulations, obtained semi-finished product;
6) top electrode preparation
5) the obtained semi-finished product of step print Ag top electrode, sinter at 600 ~ 700 DEG C, 20 minutes, obtained finished product.
Beneficial effect of the present invention:
1) (the Na with perovskite structure and strong dielectric, nonlinear, high-k is selected
0.5*(1+x)bi
0.5* (1+y)) TiO
3(wherein: 0≤x≤0.05,0≤y≤0.1) ferroelectric material and composition are BaO:B according to mol ratio
2o
3: SiO
2the glass dust doping of=3.5 ~ 5.5:2 ~ 6:0.5 ~ 2.5, obtains that to have sintering temperature low, the ferroelectric thick film that energy storage density is high.
2) the present invention adopts the technique that traditional Preparation Technique of Powders combines with screen printing technique, and flow process is simple, and cost is low, superior performance, and obtained thick film can be used as the critical material of high-power high-capacity capacitor development and application.
Accompanying drawing explanation
Fig. 1 is the XRD diffracting spectrum of high energy storage density ferroelectric thick film prepared by the embodiment of the present invention and comparative example;
Fig. 2 is the energy storage density of high energy storage density ferroelectric thick film prepared by the embodiment of the present invention and comparative example and the relation curve applying electric field;
Fig. 3 is the energy storage efficiency of high energy storage density ferroelectric thick film prepared by the embodiment of the present invention and comparative example and the relation curve applying electric field.
Specific implementation method
Embodiment 1
1) powder is prepared
11.64wt%Na will be consisted of
2cO
3(purity 99.8%), 52.62wt%Bi
2o
3(purity 99.0%), 35.74wt%TiO
2the raw material of (purity 98.0%) is placed in agate mortar, adds absolute ethyl alcohol and grinds 4 hours, dry in the drying baker of 80 DEG C after raw material is fully mixed, and the powder of oven dry adopts solid reaction process at 800 DEG C of insulations, 2 hours synthesis (Na
0.5bi
0.51) TiO
3powder, crosses 300 sieves, for subsequent use;
2) glass dust is prepared
58.96wt%BaCO will be consisted of
3(purity 99.0%), 27.57wt%HBO
3(purity 99.5%), 13.47wt%SiO
2the raw material of (purity 99%) is placed in agate mortar, add absolute ethyl alcohol and grind 4 hours, it is dry in the drying baker of 80 DEG C after raw material is fully mixed, the powder of drying is loaded in crucible, be placed in high temperature box furnace, be warming up to 1100 DEG C, be incubated 1 hour, be milled to 300 mesh sieves after shrend, obtain 4BaO-3B
2o
3-3SiO
2glass dust;
3) hearth electrode is prepared
By Ag-Pd(95/5) method of electrocondution slurry employing silk screen printing is by 300 object silk screen printings on alumina substrate, and acquisition thickness is approximately the electrode wet film of 5 microns, and after being dried by wet film, in box type furnace, 950 DEG C of insulations obtain Ag-Pd hearth electrode in 2 hours;
4) slurry is prepared
In mass ratio by 100wt%(Na
0.5bi
0.51) TiO
3powder, 3wt%4BaO-3B
2o
3-3SiO
2glass dust, 30wt% binding agent are placed in agate mortar, fully grinding 2 hours, obtained thick film ink;
5) thick film is prepared
A. by 4) the obtained thick film ink of step adopts silk screen print method to be printed on 3) Ag-Pd electrode obtained in step obtains wet film, wet film 100 DEG C of placements in drying baker are dried for 10 minutes, to be cooled to after room temperature under the pressure of 200MPa isostatic cool pressing process 10 minutes, to obtain thick film green compact;
B. thick film green compact a step obtained continue to be warming up to 800 DEG C of insulations 5 hours with 3 DEG C/min, cool to room temperature with the furnace, obtain 10 microns of thick films, obtain semi-finished product thick film after being warming up to 550 DEG C of insulations, 5 hours eliminating binding agents with 3 DEG C/min;
6) top electrode is prepared
By 5) the semi-finished product thick film for preparing of step adopts silk screen print method to print Ag top electrode, is warming up to 600 DEG C of insulations 20 minutes, with the obtained finished product of stove cooling with 3 DEG C/min.
Embodiment 2
1) powder is prepared
11.67wt%Na will be consisted of
2cO
3(purity 99.8%), 53.22wt%Bi
2o
3(purity 99.0%), 35.11wt%TiO
2the raw material of (purity 98.0%) is placed in agate mortar, adds absolute ethyl alcohol and grinds 4 hours, dry in the drying baker of 80 DEG C after raw material is fully mixed, and the powder of oven dry adopts solid reaction process at 850 DEG C of insulations, 3 hours synthesis (Na
0.51bi
0.525) TiO
3powder, crosses 300 sieves, for subsequent use;
2) glass dust is prepared
66.85wt%BaCO will be consisted of
3(purity 99.0%), 25.01wt%HBO
3(purity 99.5%), 8.14wt%SiO
2the raw material of (purity 99%) is placed in agate mortar, add absolute ethyl alcohol and grind 4 hours, it is dry in the drying baker of 80 DEG C after raw material is fully mixed, the powder of drying is loaded in crucible, be placed in high temperature box furnace, be warming up to 1250 DEG C, be incubated 1.5 hours, be milled to 300 mesh sieves after shrend, obtain 5BaO-3B
2o
3-2SiO
2glass dust;
3) hearth electrode is prepared
By Ag-Pd(95/5) method of electrocondution slurry employing silk screen printing is by 300 object silk screen printings on alumina substrate, and acquisition thickness is approximately the electrode wet film of 5 microns, and after being dried by wet film, in box type furnace, 950 DEG C of insulations obtain Ag-Pd hearth electrode in 2 hours;
4) slurry is prepared
In mass ratio by 100wt%(Na
0.51bi
0.525) TiO
3powder, 5wt%5BaO-3B
2o
3-2SiO
2glass dust, 50wt% binding agent are placed in agate mortar, fully grinding 2 hours, obtained thick film ink;
5) thick film is prepared
A. by 4) the obtained thick film ink of step adopts silk screen print method to be printed on 3) Ag-Pd electrode obtained in step obtains wet film, wet film 100 DEG C of placements in drying baker are dried for 10 minutes, to be cooled to after room temperature under the pressure of 200MPa isostatic cool pressing process 10 minutes, to obtain thick film green compact;
B. thick film green compact a step obtained continue to be warming up to 900 DEG C of insulations 8 hours with 3 DEG C/min, cool to room temperature with the furnace, obtain 50 microns of thick films, obtain semi-finished product thick film after being warming up to 550 DEG C of insulations, 5 hours eliminating binding agents with 3 DEG C/min;
6) top electrode is prepared
By 5) the semi-finished product thick film for preparing of step adopts silk screen print method to print Ag top electrode, is warming up to 600 DEG C of insulations 20 minutes, with the obtained finished product of stove cooling with 3 DEG C/min.
Embodiment 3
1) powder is prepared
11.67wt%Na will be consisted of
2cO
3(purity 99.8%), 54.20wt%Bi
2o
3(purity 99.0%), 34.13wt%TiO
2the raw material of (purity 98.0%) is placed in agate mortar, adds absolute ethyl alcohol and grinds 4 hours, dry in the drying baker of 80 DEG C after raw material is fully mixed, and the powder of oven dry adopts solid reaction process at 900 DEG C of insulations, 5 hours synthesis (Na
0.525bi
0.55) TiO
3powder, crosses 300 sieves, for subsequent use;
2) glass dust is prepared
76.38wt%BaCO will be consisted of
3(purity 99.0%), 15.87wt%HBO
3(purity 99.5%), 7.75wt%SiO
2the raw material of (purity 99%) is placed in agate mortar, add absolute ethyl alcohol and grind 4 hours, it is dry in the drying baker of 80 DEG C after raw material is fully mixed, the powder of drying is loaded in crucible, be placed in high temperature box furnace, be warming up to 1300 DEG C, be incubated 3 hours, be milled to 300 mesh sieves after shrend, obtain 6BaO-2B
2o
3-2SiO
2glass dust;
3) hearth electrode is prepared
By Ag-Pd(95/5) method of electrocondution slurry employing silk screen printing is by 300 object silk screen printings on alumina substrate, and acquisition thickness is approximately the electrode wet film of 5 microns, and after being dried by wet film, in box type furnace, 950 DEG C of insulations obtain Ag-Pd hearth electrode in 2 hours;
4) slurry is prepared
In mass ratio by 100wt%(Na
0.525bi
0.55) TiO
3powder, 20wt%6BaO-2B
2o
3-2SiO
2glass dust, 60wt% binding agent are placed in agate mortar, fully grinding 2 hours, obtained thick film ink;
5) thick film is prepared
A. by 4) the obtained thick film ink of step adopts silk screen print method to be printed on 3) Ag-Pd electrode obtained in step obtains wet film, wet film 100 DEG C of placements in drying baker are dried for 10 minutes, to be cooled to after room temperature under the pressure of 200MPa isostatic cool pressing process 10 minutes, to obtain thick film green compact;
B. thick film green compact a step obtained continue to be warming up to 950 DEG C of insulations 12 hours with 3 DEG C/min, cool to room temperature with the furnace, obtain 100 microns of thick films, obtain semi-finished product thick film after being warming up to 550 DEG C of insulations, 5 hours eliminating binding agents with 3 DEG C/min;
6) top electrode is prepared
By 5) the semi-finished product thick film for preparing of step adopts silk screen print method to print Ag top electrode, is warming up to 600 DEG C of insulations 20 minutes, with the obtained finished product of stove cooling with 3 DEG C/min.
Comparative example
1) powder is prepared
11.64wt%Na will be consisted of
2cO
3(purity 99.8%), 52.62wt%Bi
2o
3(purity 99.0%), 35.74wt%TiO
2the raw material of (purity 98.0%) is placed in agate mortar, adds absolute ethyl alcohol and grinds 4 hours, dry in the drying baker of 80 DEG C after raw material is fully mixed, and the powder of oven dry adopts solid reaction process at 850 DEG C of insulations, 3 hours synthesis (Na
0.5bi
0.5) TiO
3powder, crosses 300 sieves, for subsequent use;
2) hearth electrode is prepared
By Ag-Pd(95/5) method of electrocondution slurry employing silk screen printing is by 300 object silk screen printings on alumina substrate, and acquisition thickness is approximately the electrode wet film of 5 microns, and after being dried by wet film, in box type furnace, 950 DEG C of insulations obtain Ag-Pd hearth electrode in 2 hours;
3) slurry is prepared
In mass ratio by 100wt%(Na
0.5bi
0.51) TiO
3powder, 40wt% binding agent are placed in agate mortar, fully grinding 2 hours, obtained thick film ink;
4) thick film is prepared
A. by 3) the obtained thick film ink of step adopts silk screen print method to be printed on 2) Ag-Pd electrode obtained in step obtains wet film, wet film 100 DEG C of placements in drying baker are dried for 10 minutes, to be cooled to after room temperature under the pressure of 200MPa isostatic cool pressing process 10 minutes, to obtain thick film green compact;
B. thick film green compact a step obtained continue to be warming up to 900 DEG C of insulations 5 hours with 3 DEG C/min, cool to room temperature with the furnace, obtain 10 microns of thick films, obtain semi-finished product thick film after being warming up to 550 DEG C of insulations, 5 hours eliminating binding agents with 3 DEG C/min;
5) top electrode is prepared
By 4) the semi-finished product thick film for preparing of step adopts silk screen print method to print Ag top electrode, is warming up to 600 DEG C of insulations 20 minutes, with the obtained finished product of stove cooling with 3 DEG C/min.
Can find out that b, c, d sample of the doped-glass powder ferroelectric thick film that the present invention obtains is compared with comparative example a sample, has single perovskite structure equally as seen from Figure 1; The energy storage density of b, c, d sample of doped-glass powder ferroelectric thick film that the present invention obtains as seen from Figure 2 can reach 1.352J/cm
3, and the energy storage density maximum of the ferroelectric thick film that comparative example a sample obtains is only 0.59J/cm
3, and can find out that the maximum electric field that a sample can bear is only 275kV/cm, much smaller than the electric field strength of about the 500kV/cm that b, c, d sample can bear; Fig. 3 can find out that the energy storage efficiency of b, c, d sample of the doped-glass powder ferroelectric thick film that the present invention obtains is between 20% ~ 45%, and the energy storage efficiency of the ferroelectric thick film that comparative example a sample obtains is only about 24%.More than show: the ferroelectric thick film of the doped-glass powder in the present invention had both had higher energy storage density and higher energy storage efficiency, achieved again unleaded, can be applied in the high-power high-capacity energy storage capacitor in future unleaded field.
Claims (1)
1. the non-plumbum ferroelectric thick film of doped-glass powder high energy storage density and a preparation method, is characterized in that, comprise the steps;
1) solid-phase synthesis preparation (Na is adopted
0.5* (1+x)bi
0.5* (1+y)) TiO
3wherein: 0≤x≤0.05,0≤y≤0.1, its calcined temperature is 800 ~ 900 DEG C, and be incubated 2 ~ 5 hours, sintering temperature is 800 ~ 950 DEG C, is incubated 3 ~ 13 hours;
2) with BaCO
3, HBO
3, SiO
2for raw material, BaO:B in molar ratio
2o
3: SiO
2=3.5 ~ 5.5:2 ~ 6:0.5 ~ 2.5 mix, and its sintering temperature is 1000 ~ 1300 DEG C, is incubated 0.5 ~ 3 hour, shrend;
3) by saturating for turpentine oil alcohol and ethyl cellulose mixing according to mass ratio=10:1, the stirred in water bath 2 hours of 80 DEG C, make ethyl cellulose be dissolved in the saturating alcohol of turpentine oil completely, be cooled to room temperature stand-by;
4) by step 1) in obtained (Na
0.5* (1+x)bi
0.5* (1+y)) TiO
3powder, wherein 0≤x≤0.05,0≤y≤0.1, step 2) obtained glass dust, step 3) obtained binding agent, be that 1:0.05 ~ 0.3:0.3 ~ 0.6 is prepared according to mass ratio, in mortar, ground and mixed evenly makes thick film ink;
5) silk screen print method obtained Ag-Pd hearth electrode on alumina substrate is adopted;
6) by step 4) obtained thick film ink adopts silk screen print method to be printed on step 5) obtained wet film on obtained Ag-Pd hearth electrode;
7) by step 6) obtained wet film sinters, and sintering temperature is 800 ~ 950 DEG C, be incubated 3 ~ 13 hours, and obtain semi-finished product thick film, film thickness is 10 ~ 100 microns;
8) by step 7) obtained semi-finished product thick film adopts screen printing to brush hair and prints Ag top electrode, obtain finished product.
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Inventor after: Liu Yunying Inventor after: Zhang Le Inventor after: Zhang Liwen Inventor after: Hao Xihong Inventor after: Yang Jichun Inventor before: Hao Xihong Inventor before: Zhang Le Inventor before: Liu Yunying Inventor before: Liu Cuan Inventor before: Yang Jichun |
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