CN104193333A - Method for preparing antiferroelectric ceramics (Bi0.46Na0.46Ba0.06La0.02) ZrxTi (1-x)O3 - Google Patents
Method for preparing antiferroelectric ceramics (Bi0.46Na0.46Ba0.06La0.02) ZrxTi (1-x)O3 Download PDFInfo
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- CN104193333A CN104193333A CN201410403204.XA CN201410403204A CN104193333A CN 104193333 A CN104193333 A CN 104193333A CN 201410403204 A CN201410403204 A CN 201410403204A CN 104193333 A CN104193333 A CN 104193333A
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Abstract
The invention relates to a method for preparing a leadless antiferroelectric ceramic material (Bi0.46Na0.46Ba0.06La0.02) ZrxTi (1-x)O3(x=0.00, 0.02, 0.04, 0.06) based on the conventional solid phase reaction, for studying the phase structure and dielectric and energy-storage properties of materials. Results show that with the increase of the content of Zr, the size of grains is gradually reduced, the dielectric constant is gradually reduced and the energy storage density is firstly increased and then reduced. Due to doping of a small amount of Zr (x=0.02), the energy storage density of the ceramic material can be greatly improved, can be increased from 0.43J/cm<3> at x=0.00 to 0.77J/cm<3> at x=0.02 under an electric field of 60kV/cm, increasing by nearly 80 percent; and experiments prove that the material is an ideal leadless antiferroelectric ceramic material.
Description
Technical field
Patent of the present invention relates to one (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3the preparation method of antiferroelectric ceramics.
Background technology
Along with electronics, information and control techniques are towards development microminiaturized, highly integrated direction, and development and the use of reproducible dynamic energy device (as mobile energy devices such as the large-scale capacity regulators in electromobile, electrical network), the development of high-density energy storage capacitor is brought into schedule.As a class branch of ferroelectric material, antiferroelectric material makes it become gradually the outstanding candidate material of high-density energy storage capacitor because it has higher energy storage density.The research of antiferroelectric materials storage effect at present mainly concentrates in the lead-containing materials system of Pb-based lanthanumdoped zirconate titanates (PZT) for matrix, as Pb (Zr, Sn, the Ti) O of Sn doping
3(PZST)
[1,2]the Pb of stupalith and La doping
0.97la
0.02(Zr
0.65sn
0.24ti
0.11) O
3 [3-5]thin-film material etc.
After calendar year 2001 " ROHS/WEEE " instruction is promulgated, leadless piezoelectric material material and electrostriction material have been obtained larger progress, by contrast, fewer at the document of reporting aspect the research of lead-free anti-ferroelectric energy storage material, mainly contain Gao
[7]deng the people relaxation antiferroelectric energy storage material 0.89BiNaTiO of report recently
3-0.06BaTiO
3-0.05K
0.5na
0.5nbO
3, this paper is positioned at the [(Bi of accurate homotype phase boundary at composition
1/2na
1/2)
0.94ba
0.06] TiO
3 [8]basis on, designed a kind of antiferroelectric (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3(x=0.0,0.02,0.04,0.06) pottery, and studied its energy storage effect.
Summary of the invention
The object of patent of the present invention is to provide a kind of (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3the preparation method of antiferroelectric ceramics, is characterized in that comprising the following steps:
The preparation of step 1, raw material,
(purity is 99% to use bismuth oxide, molecular weight is 465.96), sodium carbonate (purity is 99.8%, and molecular weight is 105.99), (purity is 99% to barium carbonate, molecular weight is 197.34), titanium dioxide (purity is 98%, and molecular weight is 79.87), (purity is 99% to zirconium white, molecular weight is 123.22) and lanthanum trioxide (purity is 99.99%, and molecular weight is 325.81) as raw material.
Step 2, weigh each component,
First, according to molecular formula (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3calculate each chemical group member's amount.
Step 3, mixing
The powder of each component weighing in step 2 is poured in nylon tank and mixed, and add 2/3 place of appropriate ethanol to tank body, and use zirconia ball ball milling 6 hours on ball mill, dry, sieve, be pressed into right cylinder.
Step 4, sintering
Prepared right cylinder in step 3 is calcined to 6h at 1000 DEG C in air.Ball grinds, sieves again, and being pressed into diameter is 10 millimeters, the small cake that thickness is 1mm;
Finally, sintering 4 hours at 1150 DEG C in air calcination stove.In the both sides of small cake, then under 850 DEG C of furnace temperature, be dried 30 minutes etc. cooling rear coating silver paste, both obtained (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3antiferroelectric ceramics.
Beneficial effect:
Zr content increases, and grain-size reduces gradually, and specific inductivity reduces gradually, and directric relaxation dispersity increases, and low temperature direction is shifted at low-temperature zone specific inductivity peak, and high temperature direction is shifted at high temperature section specific inductivity peak; The increase of relaxation dispersity, is conducive to improve the anti-disruptive strength of antiferroelectric materials.And along with Zr content increases, energy storage density first increases rear minimizing.A small amount of Zr doping (x=0.02) can increase substantially ceramic energy storage density, and under the electric field of 60kV/cm, its energy storage density is by the 0.43J/cm of x=0.0
3bring up to the 0.77J/cm of x=0.02
3, almost improved 80%, than unleaded relaxation antiferroelectric 0.89[Bi
0.5na
0.5tiO
3]-0.06[BaTiO
3]-0.05[K
0.5na
0.5nbO
3] ceramic energy storage density (about 0.5J/cm
3, electric field is 60kv/cm
3) improve 54%.Suppose under form of film, its energy storage density can reach 40J/cm
3above, desirable lead-free anti-ferroelectric energy storage material will be become.
Brief description of the drawings
Below in conjunction with drawings and the embodiments, the present invention is further detailed explanation:
Fig. 1 is (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3the XRD figure spectrum of (x=0.0,0.02,0.04,0.06) pottery;
Fig. 2 is (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3the SEM surface topography of pottery: (a) x=0, (b) x=0.02, (c) x=0.04, (d) x=0.06;
Fig. 3 (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3(x=0.0,0.02,0.04,0.06) ε ' (T) for (a) of pottery under different frequency, (b) ε " (T); (c) tan δ (T), (d) (T) the Lorentz lorentz matching of curve under 10kHz of ε ';
Fig. 4 (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3ferroelectric hysteresis loop (a) x=0 of pottery under same electric field not, (b) x=0.02, (c) x=0.04, (d) x=0.06.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
A kind of (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3the preparation method of antiferroelectric ceramics, is characterized in that comprising the following steps:
The preparation of step 1, raw material,
(purity is 99% to use bismuth oxide, molecular weight is 465.96), sodium carbonate (purity is 99.8%, and molecular weight is 105.99), (purity is 99% to barium carbonate, molecular weight is 197.34), titanium dioxide (purity is 98%, and molecular weight is 79.87), (purity is 99% to zirconium white, molecular weight is 123.22) and lanthanum trioxide (purity is 99.99%, and molecular weight is 325.81) as raw material.
Step 2, weigh each component,
First, according to molecular formula (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3calculate each chemical group member's amount.
Step 3, mixing
The powder of each component weighing in step 2 is poured in nylon tank and mixed, and add 2/3 place of appropriate ethanol to tank body, and use zirconia ball ball milling 6 hours on ball mill, dry, sieve, be pressed into right cylinder.
Step 4, sintering
Prepared right cylinder in step 3 is calcined to 6h at 1000 DEG C in air.Ball grinds, sieves again, and being pressed into diameter is 10 millimeters, the small cake that thickness is 1mm;
Finally, sintering 4 hours at 1150 DEG C in air calcination stove.In the both sides of small cake, then under 850 DEG C of furnace temperature, be dried 30 minutes etc. cooling rear coating silver paste, both obtained (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3antiferroelectric ceramics.
Fig. 1 has provided (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3xRD figure spectrum after (x=0.0,0.02,0.04,0.06) ceramic post sintering.As can be seen from the figure, after 1150 DEG C of 4 hours sintering, pottery is pure Perovskite Phase structure, equates that without burnt green stone dephasign exists.Adopt JADE5.0 to carry out after structure refinement all components, gained unit cell parameters is respectively:
and then can try to achieve ceramic theoretical density according to molecular formula and unit cell volume and be respectively: ρ=5.905g/cm
3(x=0.0), ρ=5.942g/cm
3(x=0.02), ρ=5.883g/cm
3and ρ=5.949g/cm (x=0.04)
3(x=0.06).The actual density test result of pottery has shown the variation tendency identical with theoretical density, and its size is respectively: 5.609g/cm
3(x=0.0), 5.639g/cm
3(x=0.02), 5.606g/cm
3(x=0.04), 5.767g/cm
3(x=0.06).
Fig. 2 has shown (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3the SEM photo on (x=0.0,0.02,0.04,0.06) ceramics sample surface.From SEM photo, can find out, all samples all presents fine and close microstructure, and along with the increase of Zr content, the average grain size of pottery reduces gradually, is decreased to the 3.5 μ m of x=0.06 from the 5 μ m of x=0.0.
Fig. 3 (a), (b) He (c) has described respectively (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3(x=0.0,0.02,0.04,0.06) real part of permittivity of pottery under different test frequencies (ε ' (T)), imaginary part (ε " (T)) and dielectric loss (tan δ (T)) variation with temperature curve.From Fig. 3 (a), can find out, in tested temperature range, the ε ' of each component (T) exists two specific inductivity peaks on curve, and one appears at low-temperature zone, and another appears at high temperature section.Along with the increase of Zr content, low temperature direction is shifted at the specific inductivity peak of its low-temperature zone gradually, and high temperature direction is shifted at the specific inductivity peak of high temperature section.Meanwhile, there is obvious frequency dispersion feature at the specific inductivity peak of low-temperature zone, and the frequency dispersion feature at its high temperature section specific inductivity peak is very weak." (T) and on tan δ (T) curve, its low-temperature zone specific inductivity peak and high temperature section specific inductivity peak all have obvious frequency dispersal feature by contrast, at ceramic ε.For this type of phenomenon, ε ' (T) with ε " (T) or in the differing temps interval of tan δ (T) curve, may be corresponding two relaxation processes independently.The frequency dispersion of low-temperature zone is mainly caused by the relaxation of polar nano microcell (PNR), and the frequency dispersion of high temperature section may be caused by the hot activation campaign of polar nano microcell, and by means of Lorentzian can by its ε ' (T) curve separating be the contributions of high low temperature two portions, as shown in Fig. 3 (d).
Fig. 4 has provided (Bi under room temperature
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3the ferroelectric hysteresis loop (P-E) of (x=0.0,0.02,0.04,0.06) pottery under difference test electric field.As can be seen from the figure, along with the increase of Zr content, the P-E loop line of sample becomes slenderrer gradually, and its shape is more as typical relaxation ferroelectric, strength increase is worn in the resistance of sample simultaneously, is increased to 100kV/cm (x=0.06) by 60kV/cm (x=0).This phenomenon may cause the relaxation dispersity of antiferroelectric phase in sample to increase relevant with the increase of Zr content.In the time that its relaxation dispersity increases, alleviate because antiferroelectric phase is transformed into the large electric field induced strain that ferroelectric phase brings, thereby improved its anti-disruptive strength.In figure, the area of dash area has represented the density of material under extra electric field, and its large I is tried to achieve by formula (1).As can be seen from the figure, a small amount of Zr doping (x=0.02) has improved ceramic energy storage density significantly.In the time that extra electric field is 60kV/cm, its energy storage density is by the 0.43J/cm of x=0.0
3bring up to the 0.77J/cm of x=0.02
3, almost improved 80%.Its result is than the 0.89[Bi of the reports such as Gao
0.5na
0.5tiO
3]-0.06[BaTiO
3]-0.05[K
0.5na
0.5nbO
3] ceramic energy storage density (about 0.5J/cm
3, electric field is 60kV/cm) and improve 54%.Along with the continuation of Zr content increases, the energy storage density of pottery trends towards reducing, and corresponds respectively to: the 0.58J/cm of x=0.04
3, the 0.45J/cm of x=0.06
3.By experimental data is carried out to extrapolation process, can find, in the time that extra electric field reaches 100kV/cm, the energy storage density of component x=0.02 reaches 1.04J/cm
3, and the energy storage density of component x=0.0 is only 0.63J/cm
3, the energy storage density of component x=0.04 and x=0.06 is respectively 0.988J/cm
3and 0.92J/cm
3.These results show, under high electric field, along with Zr content increases, the energy storage density of pottery can correspondingly be improved.
Recent many results of study show in succession, and by means of form of film, material can sustain very large electric field and can be not breakdown, and can obtain high energy storage density.Such as, Argonne National Laboratory of the U.S. has successfully deposited the Pb of 1 micron thick left and right on nickel foil in 2009
0.92la
0.08zr
0.95ti
0.05o
3film, under the high electric field of 3500kV/cm, its energy storage density at room temperature reaches 53J/cm
3.The component of supposing x=0.02 can be made into form of film, and can sustain the electric field of 3500kV/cm, and its energy storage density will be increased to 40J/cm so
3above, thus make it likely become a kind of unleaded energy storage material of high-density with practical value.
Zr content increases, and grain-size reduces gradually, and specific inductivity reduces gradually, and directric relaxation dispersity increases, and low temperature direction is shifted at low-temperature zone specific inductivity peak, and high temperature direction is shifted at high temperature section specific inductivity peak; The increase of relaxation dispersity, is conducive to improve the anti-disruptive strength of antiferroelectric materials.And along with Zr content increases, energy storage density first increases rear minimizing.A small amount of Zr doping (x=0.02) can increase substantially ceramic energy storage density, and under the electric field of 60kV/cm, its energy storage density is by the 0.43J/cm of x=0.0
3bring up to the 0.77J/cm of x=0.02
3, almost improved 80%, than unleaded relaxation antiferroelectric 0.89[Bi
0.5na
0.5tiO
3]-0.06[BaTiO
3]-0.05[K
0.5na
0.5nbO
3] ceramic energy storage density (about 0.5J/cm
3, electric field is 60kv/cm
3) improve 54%.Suppose under form of film, its energy storage density can reach 40J/cm
3above, desirable lead-free anti-ferroelectric energy storage material will be become.
Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (1)
1. (a Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3the preparation method of antiferroelectric ceramics, is characterized in that comprising the following steps:
The preparation of step 1, raw material,
(purity is 99% to use bismuth oxide, molecular weight is 465.96), sodium carbonate (purity is 99.8%, and molecular weight is 105.99), (purity is 99% to barium carbonate, molecular weight is 197.34), titanium dioxide (purity is 98%, and molecular weight is 79.87), (purity is 99% to zirconium white, molecular weight is 123.22) and lanthanum trioxide (purity is 99.99%, and molecular weight is 325.81) as raw material;
Step 2, weigh each component,
First, according to molecular formula (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3calculate each chemical group member's amount;
Step 3, mixing
The powder of each component weighing in step 2 is poured in nylon tank and mixed, and add 2/3 place of appropriate ethanol to tank body, and use zirconia ball ball milling 6 hours on ball mill, dry, sieve, be pressed into right cylinder;
Step 4, sintering
Prepared right cylinder in step 3 is calcined to 6h at 1000 DEG C in air, and ball grinds, sieves again, and being pressed into diameter is 10 millimeters, the small cake that thickness is 1mm;
Finally, in air calcination stove, sintering 4 hours at 1150 DEG C, waits cooling rear coating silver paste in the both sides of small cake, then under 850 DEG C of furnace temperature dry 30 minutes, both (Bi
0.46na
0.46ba
0.06la
0.02) Zr
xti
(1-x)o
3antiferroelectric ceramics.
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|---|---|---|---|
| CN201410403204.XA CN104193333A (en) | 2014-08-18 | 2014-08-18 | Method for preparing antiferroelectric ceramics (Bi0.46Na0.46Ba0.06La0.02) ZrxTi (1-x)O3 |
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|---|---|---|---|
| CN201410403204.XA CN104193333A (en) | 2014-08-18 | 2014-08-18 | Method for preparing antiferroelectric ceramics (Bi0.46Na0.46Ba0.06La0.02) ZrxTi (1-x)O3 |
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|---|---|
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|---|---|---|---|---|
| CN104944944A (en) * | 2015-06-05 | 2015-09-30 | 桂林电子科技大学 | Re2x/3(Ba0.06Bi0.47Na0.47)1-xMeyTi1-yO3 leadless antiferroelectric high-energy density ceramic and preparation method thereof |
| CN104944952A (en) * | 2015-06-05 | 2015-09-30 | 桂林电子科技大学 | Rex/3(Ba0.06Bi0.47Na0.47)1-xTi1-xRxO3 leadless antiferroelectric ceramic with high energy density and preparation method thereof |
| CN106045499A (en) * | 2016-05-27 | 2016-10-26 | 西北工业大学 | Preparation method of zirconium-doped and lanthanum-doped sodium titanate-barium titanate ceramics |
| CN106396668A (en) * | 2016-09-13 | 2017-02-15 | 西安航空学院 | BNT (Sodium Bismuth Titanate)-BLT (Lanthanum-substituted Bismuth Titanate)-BMNT (Bismuth Magnesium Niobium Titanium) anti-ferroelectric energy storage ceramic and preparation method thereof |
| CN107188555A (en) * | 2017-06-22 | 2017-09-22 | 广西大学 | A kind of preparation method of ceramic target |
| CN107445616A (en) * | 2017-08-31 | 2017-12-08 | 陕西科技大学 | A kind of unleaded high pressure resistant energy storage ceramic material of strontium titanate base and preparation method thereof |
| CN109180181A (en) * | 2018-09-28 | 2019-01-11 | 西安交通大学 | A kind of unleaded relaxation antiferroelectric ceramics energy storage material and preparation method thereof |
| CN114180962A (en) * | 2021-12-30 | 2022-03-15 | 陕西科技大学 | Sodium bismuth titanate-based ceramic material with low electric field, high energy storage and ultra-fast discharge rate and preparation method thereof |
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| CN104944944B (en) * | 2015-06-05 | 2017-12-29 | 桂林电子科技大学 | Re2x/3(Ba0.06Bi0.47Na0.47)1‑xMeyTi1‑yO3Lead-free anti-ferroelectric high energy storage density ceramics and preparation method thereof |
| CN104944952A (en) * | 2015-06-05 | 2015-09-30 | 桂林电子科技大学 | Rex/3(Ba0.06Bi0.47Na0.47)1-xTi1-xRxO3 leadless antiferroelectric ceramic with high energy density and preparation method thereof |
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| CN106396668A (en) * | 2016-09-13 | 2017-02-15 | 西安航空学院 | BNT (Sodium Bismuth Titanate)-BLT (Lanthanum-substituted Bismuth Titanate)-BMNT (Bismuth Magnesium Niobium Titanium) anti-ferroelectric energy storage ceramic and preparation method thereof |
| CN106396668B (en) * | 2016-09-13 | 2019-07-19 | 西安航空学院 | A kind of BNT-BLT-BMNT anti-ferroelectric energy storage ceramic and preparation method thereof |
| CN107188555A (en) * | 2017-06-22 | 2017-09-22 | 广西大学 | A kind of preparation method of ceramic target |
| CN107445616A (en) * | 2017-08-31 | 2017-12-08 | 陕西科技大学 | A kind of unleaded high pressure resistant energy storage ceramic material of strontium titanate base and preparation method thereof |
| CN107445616B (en) * | 2017-08-31 | 2020-09-22 | 陕西科技大学 | Strontium titanate-based lead-free high-pressure-resistant energy storage ceramic material and preparation method thereof |
| CN109180181A (en) * | 2018-09-28 | 2019-01-11 | 西安交通大学 | A kind of unleaded relaxation antiferroelectric ceramics energy storage material and preparation method thereof |
| CN109180181B (en) * | 2018-09-28 | 2020-10-27 | 西安交通大学 | Lead-free relaxation antiferroelectric ceramic energy storage material and preparation method thereof |
| CN114180962A (en) * | 2021-12-30 | 2022-03-15 | 陕西科技大学 | Sodium bismuth titanate-based ceramic material with low electric field, high energy storage and ultra-fast discharge rate and preparation method thereof |
| CN114180962B (en) * | 2021-12-30 | 2023-08-18 | 深圳市荣为信科技有限公司 | Bismuth sodium titanate-based ceramic material with low electric field, high energy storage and ultrafast discharge rate and preparation method thereof |
| CN114621004A (en) * | 2022-01-26 | 2022-06-14 | 杭州电子科技大学 | High-entropy ceramic material with high energy storage density and preparation method thereof |
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