CN106396668B - A kind of BNT-BLT-BMNT anti-ferroelectric energy storage ceramic and preparation method thereof - Google Patents
A kind of BNT-BLT-BMNT anti-ferroelectric energy storage ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of BNT-BLT-BMNT anti-ferroelectric energy storage ceramics and preparation method thereof, belong to function ceramics preparation technical field, molecular formula are as follows: [(Bi1/2Na1/2)0.92Ba0.05La0.02](Mg1/ 3Nb2/3)xTi(1‑0.5x)O3, wherein x=0.01,0.03,0.05 or 0.07.Invention introduces Mg, Nb element, the crystallite dimension for solving anti-ferroelectric energy storage ceramic in the prior art is bigger than normal and be unevenly distributed, and energy-storage property is undesirable, to the problem of electric field reaction sensitivity difference.
Description
Technical field
The invention belongs to function ceramics preparation technical field, be related to a kind of BNT-BLT-BMNT anti-ferroelectric energy storage ceramic and its
Preparation method.
Background technique
In recent years, with the high speed development of science and technology, in order to meet growing electrical energy demands, there is an urgent need to develop one kind
Efficiently, high performance power storage and transition material.It is a large amount of that power storage capacitor requirement functional material can satisfy accumulation
Energy, and can spark.Therefore, energy storage material has played vital effect in pulse power application.Therefore, unleaded
The development and application of anti-ferroelectric ceramic material are increasingly becoming the hot spot of research.In numerous lead-free anti-ferroelectric ceramic systems, BNT-BT
Matrix system is to be applied to high energy storage density high power capacity because it has anti-ferroelectricity in specific component and temperature range
One of ideal candidates material of device, for BNT-BT sill due to its superior electric property, the antiferroelectric materials is close in high-energy
Spend ceramic capacitor in have very big application potential, so its have on mobile electronic device and electric automobile it is wide
Application prospect.
Summary of the invention
In order to achieve the above object, the present invention provides a kind of BNT-BLT-BMNT anti-ferroelectric energy storage ceramic, introduces Mg, Nb
Element, the crystallite dimension for solving anti-ferroelectric energy storage ceramic in the prior art is bigger than normal and be unevenly distributed, and energy-storage property is undesirable,
To the problem of electric field reaction sensitivity difference.
It is another object of the invention to provide a kind of preparation methods of above-mentioned anti-ferroelectric energy storage ceramic.
The technical scheme adopted by the invention is that a kind of BNT-BLT-BMNT anti-ferroelectric energy storage ceramic, molecular formula are as follows:
[(Bi1/2Na1/2)0.92Ba0.05La0.02](Mg1/3Nb2/3)xTi(1-0.5x)O3, wherein x=0.01,0.03,0.05 or 0.07.
Another technical solution of the present invention is a kind of preparation method of BNT-BLT-BMNT anti-ferroelectric energy storage ceramic, feature
It is, specifically follows the steps below:
Step 1, according to molecular formula are as follows: [(Bi1/2Na1/2)0.92Ba0.05La0.02](Mg1/3Nb2/3)xTi(1-0.5x)O3, wherein x
=0.01,0.03,0.05 or 0.07, calculate the requirement of each raw material, required raw material are as follows: titanium dioxide, niobium oxide, magnesia,
Lanthana, sodium carbonate, bismuth oxide and barium carbonate；It is weighed with electronic balance, weighing is accurate to after decimal point 3；
Step 2, load weighted each raw material is poured into nylon tank, the zirconia ball of 1/10 volume of nylon tank body is added, then
It pours at high-purity (purity 99.9%) ethyl alcohol to the 2/3 of nylon tank body, ball milling 24 hours on ball mill, dry later, sieving,
A monolith cylindrical body is pressed on press machine, then 900 DEG C of calcining 6h under atmospheric environment；
Step 3, ball milling is for 24 hours at powder again, and sieving, it is 10mm that diameter is pressed on cold isostatic press, with a thickness of the small of 1mm
Cake；Small cake is buried with the powder of same composition, 6h is sintered at 1200 DEG C in air calcination stove, is cooled to room
Temperature to get.
Of the invention to be further characterized in that, further, the purity of titanium dioxide is 98% in step 1, the purity of niobium oxide
It is 99%, the purity of magnesia is 99.8%, and the purity of lanthana is 99.99%, and the purity of sodium carbonate is 99.8%, bismuth oxide
Purity be 99%, the purity of barium carbonate is 99%.
Further, in step 2, the zirconia ball quantity of diameter 2mm and diameter 5mm respectively accounts for half in zirconia ball.
The beneficial effects of the present invention are: by introducing Mg, Nb element, the crystallite dimension of present invention ceramics becomes smaller, is distributed more
Uniformly, combined coefficient can be significantly improved；Because of Mg2+And Nb5+Ionic radius be greater thanIonic radius, with
?Addition lead to sample distortion of lattice of the invention.
With the addition of Mg, Nb element, facilitates sample of the invention and change to antiferroelectric ceramics.With the increase of x value,
Maximum polarization PmaxWith remanent polarization PrBetween difference be more and more obvious, illustrate the energy storage of electroceramics of the present invention
It can become better and better, the addition for further relating to Mg, Nb element helps to improve the energy-storage property of lead-free anti-ferroelectric ceramics.In addition,
Ceramic systems of the present invention are quick on the draw to electric field, with the variation of electric field, corresponding stress induction can be generated, in piezoelectric property
Aspect is also showed.
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
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the XRD spectrum of embodiment 1-4.
Fig. 2 is the enlarged drawing at (111) peak and (200) peak in Fig. 1.
Fig. 3 is the lattice constant of embodiment 1-4 with the change curve of x value.
Fig. 4 a is the SEM surface topography map of embodiment 1.
Fig. 4 b is the SEM surface topography map of embodiment 2.
Fig. 4 c is the SEM surface topography map of embodiment 3.
Fig. 4 d is the SEM surface topography map of embodiment 4.
Fig. 5 is ferroelectric hysteresis loop of the embodiment 1-4 under room temperature and phase same electric field.
Fig. 6 is embodiment 1-4 maximum polarization PmaxWith remanent polarization PrDifference curve.
Fig. 7 is the stress of embodiment 1-4 with the change curve of electric field.
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.
Embodiment 1,
The present invention is prepared using two step solid state reactions, is specifically followed the steps below:
Step 1, molecular formula [(Bi according to the invention1/2Na1/2)0.92Ba0.05La0.02](Mg1/3Nb2/3)xTi(1-0.5x)O3,
Wherein x=0.01 calculates the requirement of each raw material, required raw material are as follows: the titanium dioxide that purity 98%, molecular weight are 79.87,
The niobium oxide that purity is 99%, molecular weight is 265.8098, the magnesia that purity 99.8%, molecular weight are 40.3, purity are
99.99%, the lanthana that molecular weight is 325.81, the sodium carbonate that purity 99.8%, molecular weight are 105.99, purity are
99%, the bismuth oxide and purity that molecular weight is 465.96 be 99%, the barium carbonate that molecular weight is 197.34；It is carried out with electronic balance
It weighs, weighing is accurate to after decimal point 3；
Step 2, load weighted each raw material is poured into nylon tank, the zirconia ball of 1/10 volume of nylon tank body, oxygen is added
The zirconia ball quantity for changing diameter 2mm and diameter 5mm in zirconium ball respectively accounts for half, then pours into the ethyl alcohol that volumetric concentration is 99.9% extremely
At the 2/3 of nylon tank body, ball milling 24 hours on ball mill, dry later, sieving is pressed into a monolith cylinder on press machine
Body, then 900 DEG C of calcining 6h under atmospheric environment；
Step 3, ball milling is for 24 hours at powder again, and sieving, it is 10mm, with a thickness of the small of 1mm that diameter is pressed on cold isostatic press
Cake, in order to study test；In order to reduce the volatilization of raw material in sample sintering procedure, with the powder of same composition by small cake
Burial is got up, and is sintered 6h at 1200 DEG C in air calcination stove, be cooled to room temperature to get.
Embodiment 2,
In addition to x value in step 1, other steps are same as Example 1；
Step 1, molecular formula [(Bi according to the invention1/2Na1/2)0.92Ba0.05La0.02](Mg1/3Nb2/3)xTi(1-0.5x)O3,
Wherein x=0.03 calculates the requirement of each raw material, is weighed with electronic balance, and weighing is accurate to after decimal point 3.
Embodiment 3,
In addition to x value in step 1, other steps are same as Example 1；
Step 1, molecular formula [(Bi according to the invention1/2Na1/2)0.92Ba0.05La0.02](Mg1/3Nb2/3)xTi(1-0.5x)O3,
Wherein x=0.05 calculates the requirement of each raw material, is weighed with electronic balance, and weighing is accurate to after decimal point 3.
Embodiment 4,
In addition to x value in step 1, other steps are same as Example 1；
Step 1, molecular formula [(Bi according to the invention1/2Na1/2)0.92Ba0.05La0.02](Mg1/3Nb2/3)xTi(1-0.5x)O3,
Wherein x=0.07 calculates the requirement of each raw material, is weighed with electronic balance, and weighing is accurate to after decimal point 3.
In order to keep result of study more obvious, x is great-jump-forward value in embodiment 1-4, below to embodiment 1-4 preparation
Ceramic sample is tested for the property:
It is tested by the density of Archimedes's drainage ceramics, using X-ray diffractometer (XRD, X ' Pert
PROMPD, Philips, Eindhoven, Netherlands) phase structure of ceramics is analyzed；The microstructure of ceramics is adopted
It is observed with field emission scanning electron microscope (JEOL-6700F, Japan Electron Co., Tokyo, Japan).?
Two cylindrical surfaces coat silver paste to sample up and down, then dry 30 minutes at 850 DEG C in drying oven, then polish off sample with sand paper
Silver paste on product cylindrical surface carries out various electric performance tests as electrode.Dielectric response uses precise impedance analyzer
(4294A, Agilent, CA, USA) is tested, and temperature control uses temperature controller (TP94, Linkam, Surrey, UK), excitation
Voltage is 500mV/mm, and test frequency range is 100Hz to 1MHz, and the temperature range of data acquisition is 300K to 700K, heating
Rate is set as 5 DEG C/min；Sample ferroelectric hysteresis loop (P-E) using ferroelectricity analyzer TF2000 (AixACCT, Aachen,
Germany it) is tested, test frequency 1Hz.
The analysis of said sample the performance test results:
1. phase structure is analyzed:
As shown in Figure 1, all components of the present invention are pure perovskite phase structure, the miscellaneous phases such as no green stone of coke are generated.It can from Fig. 2
To find out, with the increase of x value, diffraction maximum is gradually mobile to low angle direction, explanation Addition lead to distortion of lattice, because of Mg2+And Nb5+Ionic radius be greater thanIon half
Caused by diameter.There is scholar to think, be mainly counterfeit cubic crystal structure in BNT-BT based solid solution ceramic material, because due to doping
The addition of element will lead to lattice and slight distortion occur.From figure 3, it can be seen that lattice constant becomes larger as the increase of x value has
Trend, this testing result have exactly been confirmed in Fig. 2, Mg2+And Nb5+Ionic radius be greater than Ti4+Ionic radius thing
It is real.
2. microstructure morphology is analyzed:
Can be seen that the increase (i.e. the increase of Mg, Nb constituent content) with x value from Fig. 4 a-4d, present invention ceramics it is big
Block crystal grain gradually becomes smaller.As shown in Fig. 4 b-4d, as x >=0.03, the grain size in present invention ceramics tends to uniformly, average
About 4 μm；With the increase of x value, the grain size and changes in distribution trend of present invention ceramics slow down, and illustrate that Mg, Nb element help
In the grain size and distribution situation that improve present invention ceramics, the addition of Mg, Nb element can significantly improve effective conjunction of the ceramics
At.
As shown in figure 5, ferroelectric hysteresis loop of the present invention under room temperature and phase same electric field is typical ferroelectric hysteresis loop map, occur
Transition stage significantly from ferroelectric to antiferroelectric.From fig. 5, it can be seen that as x≤0.03, which is
Typical ferroelectric hysteresis loop；As x >=0.05, which there is " necking down " with the increase of electric field strength
Phenomenon, curved intermediate part point are gradually drawn close narrowed, are intended to be changed into antiferroelectric state, illustrate that the addition of Mg, Nb element has
Help BNT-BT ferroelectric ceramics to change to antiferroelectric ceramics.
Fig. 6 shows the maximum polarization P of ceramics of the inventionmaxWith remanent polarization PrBetween difference.From Fig. 6
As can be seen that with the increase of x value, maximum polarization PmaxWith remanent polarization PrBetween difference be more and more obvious, say
The energy-storage property of the bright ceramics is become better and better.Illustrate that the addition of Mg, Nb element helps to improve the energy-storage property of system ceramics.
Fig. 7 shows the stress of ceramics of the invention with the change curve of electric field.From figure 7 it can be seen that as x=0.07,
Maximum bipolarity stress is 0.358%, and as x=0.05, maximum bipolarity stress is reduced to rapidly 0.156%, later with x
Value further decreases, and maximum bipolarity stress variation is unobvious, and respectively 0.151%, 0.130%.By curve feature come
It sees, as x≤0.03, curve has shown " W type " butterfly-like curve specific to typical ferroelectric, as x >=0.05,
Curve has shown V-type shape curve specific to typical relaxation ferroelectric.The results show that ceramic systems of the present invention react electric field
It is sensitive, with the variation of electric field, corresponding stress induction can be generated, is also showed in terms of piezoelectric property.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention
It is interior.
Claims (2)
1. a kind of preparation method of BNT-BLT-BMNT anti-ferroelectric energy storage ceramic, which is characterized in that specifically according to the following steps into
Row:
Step 1, according to molecular formula: [(Bi1/2Na1/2)0.92Ba0.05La0.02](Mg1/3Nb2/3)xTi(1-0.5x)O3, wherein x=0.05,
Calculate the requirement of each raw material；Wherein, required raw material are as follows: titanium dioxide, niobium oxide, magnesia, lanthana, sodium carbonate, oxidation
Bismuth and barium carbonate；It is weighed with electronic balance, weighing is accurate to after decimal point 3；
Step 2, load weighted each raw material is poured into nylon tank, the zirconia ball of 1/10 volume of nylon tank body is added, then poured into
At the ethyl alcohol to the 2/3 of nylon tank body that volumetric concentration is 99.9%, ball milling 24 hours on ball mill, dry later, sieving,
A monolith cylindrical body is pressed on press machine, then 900 DEG C of calcining 6h under atmospheric environment；
Step 3, ball milling is for 24 hours at powder again, and sieving, it is 10mm that diameter is pressed on cold isostatic press, with a thickness of the roundlet of 1mm
Cake；Small cake is buried with the powder of same composition, 6h is sintered at 1200 DEG C in air calcination stove, is cooled to room temperature,
To obtain the final product；
In the step 2, the zirconia ball quantity of diameter 2mm and diameter 5mm respectively accounts for half in zirconia ball.
2. a kind of preparation method of BNT-BLT-BMNT anti-ferroelectric energy storage ceramic according to claim 1, which is characterized in that
The purity of titanium dioxide is 98% in the step 1, and the purity of niobium oxide is 99%, and the purity of magnesia is 99.8%, oxidation
The purity of lanthanum is 99.99%, and the purity of sodium carbonate is 99.8%, and the purity of bismuth oxide is 99%, and the purity of barium carbonate is 99%.
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| CN104193333A (en) * | 2014-08-18 | 2014-12-10 | 曹静 | Method for preparing antiferroelectric ceramics (Bi0.46Na0.46Ba0.06La0.02) ZrxTi (1-x)O3 |
| CN104891989A (en) * | 2015-05-14 | 2015-09-09 | 桂林电子科技大学 | Srx(Bi0.47Na0.47Ba0.06)1-xMxTi1-xO3 high energy density ceramic and preparation method thereof |
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| CN104193333A (en) * | 2014-08-18 | 2014-12-10 | 曹静 | Method for preparing antiferroelectric ceramics (Bi0.46Na0.46Ba0.06La0.02) ZrxTi (1-x)O3 |
| CN104891989A (en) * | 2015-05-14 | 2015-09-09 | 桂林电子科技大学 | Srx(Bi0.47Na0.47Ba0.06)1-xMxTi1-xO3 high energy density ceramic and preparation method thereof |
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