CN108314443A - A kind of high energy storage density antiferroelectric thick film and preparation method thereof - Google Patents
A kind of high energy storage density antiferroelectric thick film and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to technical field of functional ceramics, a kind of high energy storage density antiferroelectric thick film and preparation method thereof is disclosed, the group of the antiferroelectric materials becomes (Pb0.98La0.02)(Sn1‑xZrx)0.998O3, wherein 0.4≤x≤0.5, antiferroelectric thick film of the invention has special ferroelectric hysteresis loop structure, not only has big resistance to breakdown electric field and phase transition electric field, while having larger 51.8 μ C/cm of polarization intensity2, make it have higher 4.2~6.9J/cm of energy storage density3, this has very important significance for developing and preparing high energy storage density antiferroelectric materials.
Description
Technical field
The invention belongs to technical field of functional ceramics, more particularly, to a kind of high energy storage density antiferroelectric thick film and its
Preparation method.
Background technology
Energy storage density is developed in fast development with Pulse Power Techniques and the active demand to great power pulse power source
The impulse capacitor high, discharge current is big, the velocity of discharge is fast, output power is high has become current PRF power technology area research
Emphasis.The adjacent dipole of reversed arrangement can invert under electric field action in antiferroelectric, induce as ferroelectric, and lead
Polarization intensity and dielectric constant is caused to mutate, the applied electric field of removal, the then ferroelectric state being induced returns to anti-iron again
Electric state, reversed arrangement, remanent polarization zero, stored charge are come out dipole by whole quick releases once again, this
Characteristic makes antiferroelectric materials have unique advantage in high power density capacitor application field.Since 2010, Hen Duoyan
Mechanism is studied carefully all using pulse power electricity container as priority research areas.
The energy storage formula of antiferroelectric materials can be indicated with following formula (1)：
Wherein, PmaxAnd PrFor maximum polarization and remanent polarization, dP is the polarization variable under electric field action, Vact
It is dielectric effective volume, U is stored gross energy, square directly proportional to application electric field, therefore improves breakdown electric field
It is to improve the important channel of energy storage density, while saturated polarization also has a major impact energy storage density.Higher energy storage is close
Degree is conducive to the miniaturization and micromation of device, in the case of limited bulk, realize high-power output.
Ca-Ti ore type Pb based antiferroelectric energy storage materials are studied the most extensive, include mainly PbZrO3, Pb (Zr, Ti) O3,
Pb(Zr,Sn,Ti)O3System and its related doping vario-property material.The component of material has a significant impact to energy-storage property, by right
Ion doping, component change to improve the shape of ferroelectric hysteresis loop, can improve energy storage density.It is to prepare dielectric material to roll membrane process
A kind of important process of material, there is important application in preparing piezoelectric material and metal film.With silk-screen printing technique and stream
Prolong that technology utilization its own gravity is different, roll film be using between two idler wheels extruding and shearing force sample is squeezed repeatedly
Pressure, final molding, sample consistency higher, breakdown performance higher.
It is relatively fewer for the research of ferroelectric hysteresis loop shape, research object according to the present invention, and titanium elements are not contained,
It is the solid solution of lead zirconates and lead stannate so that it has more unique dielectric polarization characteristic, the polarization intensity of bigger and energy storage
Density.
Invention content
In order to solve above-mentioned the shortcomings of the prior art, a kind of antiferroelectric thick film of high energy storage density is provided.
The one of the present invention is designed to provide the anti-iron of above-mentioned graphene-containing watersoluble baking type conductive coating high energy storage density
The preparation method of electric thick film.
The purpose of the present invention is realized by following technical proposals：
A kind of high energy storage density antiferroelectric thick film, be by lanthana, lead oxide, zirconium oxide, tin oxide and titanium oxide according to
Ball milling is carried out after stoichiometric ratio dispensing, adhesive is added after pre-burning, through roughing formin blank, through being sintered plated electrode after dumping
It is made, molecular formula is (Pb0.98La0.02)(Sn1-xZrx)0.998O3, wherein 0.4≤x≤0.5.
Preferably, the molecular formula of the high energy storage density antiferroelectric thick film is (Pb0.98La0.02)(Sn1-xZrx)0.998O3,
Wherein 0.43≤x≤0.45.
Preferably, described adhesive is PVA or PVB, a concentration of 8~10wt.% of described adhesive.
The preparation method of above-mentioned high energy storage density antiferroelectric thick film, comprises the following specific steps that：
S1. lanthana, lead oxide, zirconium oxide, tin oxide and titanium oxide are carried out dispensing according to stoichiometric ratio dispensing
Ball milling；
S2. the material after ball milling is dried, in 900~950 DEG C of pre-burnings, ball milling again after powder after pre-burning is smashed takes out
Afterwards, sieving is used after drying；
S3. adhesive, the roughing repeatedly on roll forming machine is added in the powder after step S2 sievings, then finish rolling forms biscuit
Piece；
S4. biscuit piece is placed in stove and is warming up to 600~700 DEG C of dumpings, kept the temperature；
S5. the biscuit piece after dumping obtained by step S4 is sintered at 1000~1260 DEG C, is cooled to room temperature taking-up naturally, plated
High energy storage density antiferroelectric thick film is made in gold electrode.
Preferably, the rotating speed of ball milling described in step S1 is 300~350 revs/min, time of the ball milling is 6~
12h。
Preferably, the aperture sieved described in step S2 is 120~200 mesh, and the temperature of the drying is 80~150 DEG C, institute
The time for stating pre-burning is 2~4h, and the time of the ball milling is 6~12h.
Preferably, adhesive described in step S3 is 15~30% of the powder quality after sieving, the time of the roughing
For 1~2h.
Preferably, the rate to heat up described in step S4 is 1~3 DEG C/min, and the time of the heat preservation is 2~5h.
Compared with prior art, the invention has the advantages that：
1. in room temperature, full charge reversible antiferroelectric-ferroelectric phase can occur off field for the antiferroelectric thick film material of the present invention
Become.
2. the antiferroelectric thick film of the present invention has larger switching electric field, antiferroelectric thick film material compactness is good, resistance to breakdown
Performance is good, and due to special phase-change characteristic, saturated polarization is larger, and saturated polarization is larger, reaches 51.8 μ C/
cm2, therefore there is higher energy storage density, energy storage reaches 4.2~6.9J/cm3, for realizing that high power discharge is significant.
Description of the drawings
Fig. 1 is 1 (Pb of embodiment0.98La0.02)(Sn0.50Zr0.50)0.998O3Ferroelectric hysteresis loop.
Fig. 2 is 2 (Pb of embodiment0.98La0.02)(Sn0.60Zr0.40)0.998O3Ferroelectric hysteresis loop.
Fig. 3 is 1 (Pb of embodiment0.98La0.02)(Sn0.50Zr0.50)0.998O3Surface SEM photograph.
Specific implementation mode
The content further illustrated the present invention with reference to specific embodiment, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagent, methods and apparatus.
Embodiment 1
1. according to stoichiometric ratio (Pb0.98La0.02)(Sn0.50Zr0.50)0.998O3By lead oxide, lanthana, zirconium oxide and
Tin oxide carries out weighing dispensing, and the material prepared is put into ball grinder, Ball-milling Time 12h；
2. take out drying after ball milling, the pre-burning 2h at 900 DEG C, then ball milling 12h again, sieving.30%PVA is added to bond
The square piece of 10mm*10mm is cut into agent, the first repeatedly roughing 1h on roll forming machine, last finish rolling to 0.1mm；
3. be put into stove in 600 DEG C of dumpings 4 hours, 1 DEG C/min of heating rate, finally by the biscuit piece after dumping, as
In closed alumina dry pot, appropriate (Pb is added in bottom0.97La0.02)(Zr0.29Sn0.65Ti0.06)O3Powder, to avoid lead
It is lost in；
4. then the alumina dry pot for filling biscuit piece is put into sintering furnace, it is sintered at 1100 DEG C, after the completion of sintering,
One layer of gold electrode is plated using observing and controlling sputter, the ferroelectric hysteresis loop of the measured component is as shown in Figure 1, show special polarization spy
Property, energy storage density reaches 4.2J/cm3.For its Surface Microstructure as shown in figure 3, crystal grain is smaller, size uniform is fine and close, is its tool
There is the major reason of high breakdown electric field.
A kind of high energy storage density antiferroelectric thick film prepared by the above method, molecular formula are (Pb0.98La0.02)
(Sn0.57Zr0.43)0.998O3。
Embodiment 2
1. according to (Pb0.98La0.02)(Sn0.60Zr0.40)0.998O3Stoichiometric ratio, by lead oxide, lanthana, zirconium oxide and
Tin oxide carries out weighing dispensing, and the material prepared is put into ball grinder, ratio of grinding media to material 3：1, add deionized water to go at 2/3, ball milling
Time 12h；
2. take out drying after ball milling, the pre-burning 2h at 900 DEG C, then ball milling 12h again, sieving；30%PVA is added to bond
The square piece of 10mm*10mm is cut into agent, the first repeatedly roughing 1h on roll forming machine, last finish rolling to 0.1mm；
3. being put into stove in 600 DEG C of dumping 4h, 1 DEG C/min of heating rate, finally by the biscuit piece after dumping, as close
In the alumina dry pot closed, appropriate (Pb is added in bottom0.98La0.02)(Sn0.60Zr0.40)0.998O3Powder, to avoid the stream of lead
It loses；
4. then the alumina dry pot for filling biscuit piece is put into sintering furnace, it is sintered at 1100 DEG C, after the completion of sintering,
One layer of gold electrode is plated using observing and controlling sputter.Its ferroelectric hysteresis loop characteristic is as shown in Fig. 2, show special polarization characteristic, energy storage
Density reaches 6.9J/cm3。
A kind of high energy storage density antiferroelectric thick film prepared by the above method, molecular formula are (Pb0.98La0.02)
(Sn0.57Zr0.43)0.998O3。
Embodiment 3
Using the method for embodiment 1, by lanthana, lead oxide, zirconium oxide, tin oxide and titanium oxide are according to stoichiometric ratio
Ball milling is carried out after dispensing, adhesive is added after pre-burning, through roughing formin blank, through being sintered high made from plated electrode store up after dumping
Energy density antiferroelectric thick film, molecular formula are (Pb0.98La0.02)(Sn0.57Zr0.43)0.998O3。
Embodiment 4
Using the method for embodiment 1, by lanthana, lead oxide, zirconium oxide, tin oxide and titanium oxide are according to stoichiometric ratio
Ball milling is carried out after dispensing, adhesive is added after pre-burning, through roughing formin blank, through being sintered high made from plated electrode store up after dumping
Energy density antiferroelectric thick film, molecular formula are (Pb0.98La0.02)(Sn0.55Zr0.45)0.998O3。
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitute, combination and simplify,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (8)
1. a kind of high energy storage density antiferroelectric thick film, which is characterized in that the high energy storage density antiferroelectric thick film be by lanthana,
Adhesive is added according to ball milling is carried out after stoichiometric ratio dispensing in lead oxide, zirconium oxide, tin oxide and titanium oxide after pre-burning, warp
Roughing formin blank is made through being sintered plated electrode after dumping, and molecular formula is (Pb0.98La0.02)(Sn1-xZrx)0.998O3,
In 0.4≤x≤0.5.
2. according to the high energy storage density antiferroelectric thick film described in claim 1, which is characterized in that the high energy storage density is anti-
The molecular formula of ferroelectric thick film is (Pb0.98La0.02)(Sn1-xZrx)0.998O3, wherein 0.43≤x≤0.45.
3. according to the high energy storage density antiferroelectric thick film described in claim 1, which is characterized in that the adhesive is PVA
Or PVB, a concentration of 8~10wt.% of the adhesive.
4. the preparation method of the high energy storage density antiferroelectric thick film according to claim any one of 1-3, which is characterized in that
It comprises the following specific steps that：
S1. by lanthana, lead oxide, zirconium oxide, tin oxide and titanium oxide according to stoichiometric ratio dispensing, dispensing is subjected to ball
Mill；
S2. the material after ball milling is dried, in 900~950 DEG C of pre-burnings, ball milling again after powder after pre-burning is smashed after taking-up, dries
Sieving is used after dry；
S3. the powder after step S2 sieving is added adhesive, the roughing repeatedly on roll forming machine, then finish rolling formin blank；
S4. biscuit piece is placed in stove and is warming up to 600~700 DEG C of dumpings, kept the temperature；
S5. the biscuit piece after dumping obtained by step S4 is sintered at 1000~1260 DEG C, is cooled to room temperature taking-up, gold-plated electricity naturally
High energy storage density antiferroelectric thick film is made in pole.
5. according to the preparation method of the high energy storage density antiferroelectric thick film described in claim 4, which is characterized in that in step S1
The rotating speed of the ball milling is 300~350 revs/min, and the time of the ball milling is 6~12h.
6. according to the preparation method of the high energy storage density antiferroelectric thick film described in claim 4, which is characterized in that in step S2
The aperture of the sieve is 120~200 mesh, and the temperature of the drying is 80~150 DEG C, time of the pre-burning is 2~
The time of 4h, the ball milling are 6~12h.
7. according to the preparation method of the high energy storage density antiferroelectric thick film described in claim 4, which is characterized in that in step S3
The adhesive is 15~30% of the powder quality after sieving, and the time of the roughing is 1~2h.
8. according to the preparation method of the high energy storage density antiferroelectric thick film described in claim 4, which is characterized in that in step S4
The rate of the heating is 1~3 DEG C/min, and the time of the heat preservation is 2~5h.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110342925A (en) * | 2019-06-25 | 2019-10-18 | 同济大学 | A kind of anti-ferroelectric ceramic material and preparation method thereof |
| CN111548154A (en) * | 2020-05-14 | 2020-08-18 | 内蒙古科技大学 | High-energy-storage-density low-lead-zirconate-titanate-based antiferroelectric ceramic and preparation method thereof |
| CN111574198A (en) * | 2020-05-14 | 2020-08-25 | 内蒙古科技大学 | High-energy-storage lead zirconate-based antiferroelectric multilayer ceramic capacitor and preparation method thereof |
| CN111718194A (en) * | 2020-07-02 | 2020-09-29 | 内蒙古科技大学 | Antiferroelectric material, preparation method thereof and capacitor containing antiferroelectric material |
| CN111960820A (en) * | 2020-07-31 | 2020-11-20 | 东莞东阳光科研发有限公司 | Piezoelectric crystal material and preparation method thereof |
| CN113429203A (en) * | 2021-07-21 | 2021-09-24 | 广东工业大学 | Lead zirconate stannate thick film ceramic material with high breakdown electric field resistance and preparation method thereof |
| CN114751735A (en) * | 2022-03-03 | 2022-07-15 | 常州大学 | Dielectric energy storage ceramic powder, preparation method and application thereof in ceramic membrane |
| CN115872735A (en) * | 2022-11-18 | 2023-03-31 | 广东工业大学 | Zirconium tin hafnate lanthanum lead ceramic and preparation method and energy storage application thereof |
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Cited By (10)
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| CN110342925A (en) * | 2019-06-25 | 2019-10-18 | 同济大学 | A kind of anti-ferroelectric ceramic material and preparation method thereof |
| CN110342925B (en) * | 2019-06-25 | 2021-10-08 | 同济大学 | Antiferroelectric ceramic material and preparation method thereof |
| CN111548154A (en) * | 2020-05-14 | 2020-08-18 | 内蒙古科技大学 | High-energy-storage-density low-lead-zirconate-titanate-based antiferroelectric ceramic and preparation method thereof |
| CN111574198A (en) * | 2020-05-14 | 2020-08-25 | 内蒙古科技大学 | High-energy-storage lead zirconate-based antiferroelectric multilayer ceramic capacitor and preparation method thereof |
| CN111718194A (en) * | 2020-07-02 | 2020-09-29 | 内蒙古科技大学 | Antiferroelectric material, preparation method thereof and capacitor containing antiferroelectric material |
| CN111960820A (en) * | 2020-07-31 | 2020-11-20 | 东莞东阳光科研发有限公司 | Piezoelectric crystal material and preparation method thereof |
| CN113429203A (en) * | 2021-07-21 | 2021-09-24 | 广东工业大学 | Lead zirconate stannate thick film ceramic material with high breakdown electric field resistance and preparation method thereof |
| CN114751735A (en) * | 2022-03-03 | 2022-07-15 | 常州大学 | Dielectric energy storage ceramic powder, preparation method and application thereof in ceramic membrane |
| CN115872735A (en) * | 2022-11-18 | 2023-03-31 | 广东工业大学 | Zirconium tin hafnate lanthanum lead ceramic and preparation method and energy storage application thereof |
| CN115872735B (en) * | 2022-11-18 | 2024-01-16 | 广东工业大学 | Zirconium tin hafnium lanthanum lead acid ceramic, preparation method and energy storage application thereof |
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Application publication date: 20180724 |