CN106187165A - A kind of high energy storage density medium ceramic material and preparation method thereof - Google Patents

A kind of high energy storage density medium ceramic material and preparation method thereof Download PDF

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CN106187165A
CN106187165A CN201610540311.6A CN201610540311A CN106187165A CN 106187165 A CN106187165 A CN 106187165A CN 201610540311 A CN201610540311 A CN 201610540311A CN 106187165 A CN106187165 A CN 106187165A
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郑兴华
肖腾
刘洋
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Fuzhou University
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Abstract

The invention discloses a kind of high energy storage density medium ceramic material and preparation method thereof.This ceramic material is to be composited by BST pottery mixed powder and MAS glass dust, and the consumption of MAS glass dust is the 0.2% ~ 10% of BST pottery mixed powder quality；Described MAS glass dust is consisting of MgO Al2O3‑SiO2；Described BST pottery mixed powder is to be the Ba of 0.1 0.5 by x value1‑xSrxTiO3In powder body multiple powder body equimolar mixing, ball milling and obtain.Compared with prior art, the energy-storing dielectric ceramic that prepared by the present invention has high (>1600 of dielectric constant), dielectric loss low (<0.02), the high (>18.0kV/mm of breakdown field strength), the high (>2.50J/cm of energy storage density3) and 55 125 DEG C in the range of change in dielectric constant rate 13.0% 5.0% advantage, be with a wide range of applications in pulse power energy-storage system.

Description

A kind of high energy storage density medium ceramic material and preparation method thereof
Technical field
The invention belongs to field of dielectric energy storage material, be specifically related to a kind of high energy storage density medium ceramic material and system thereof Preparation Method.
Technical background
In recent years in electronics industry, high energy storage density device is increasingly paid close attention to by people, studies new high storage Energy device is extremely urgent.Being compared to traditional energy storage device, dielectric capacitor utilizes polarization charge to store electric energy, and it fills Discharge rate and the discharge energy density several orders of magnitude higher than traditional energy storage device.It addition, it has more preferable stability, Technical field of pulse power, hybrid vehicle aspect demand is relatively big, has the highest application prospect.But current electrolyte The energy storage density of energy-storage capacitor does not reaches the most far away the demand of application, and the energy storage density the most how improving dielectric substance becomes For research emphasis.
In dielectric energy storage material, its energy storage density is usedRepresent, wherein ε0For permittivity of vacuum, εrFor relative dielectric constant, E is electric field intensity.Can be seen that the energy storage density of dielectric energy storage material is determined by two factors: Dielectric constant and breakdown field strength.The dielectric substance of capacitor energy storage device mainly has TiO at present2、BaTiO3、Ba1- xSrxTiO3Deng, all there is higher dielectric constant, especially Ba1-xSrxTiO3(BST) possesses high dielectric constant and low because of it Dielectric loss, has obtained studying widely.But, Ba1-xSrxTiO3The dielectric strength of pottery is generally below 8kV/mm, is unfavorable for Obtain higher energy storage density.It addition, single component Ba1-xSrxTiO3Ceramic dielectric constant with temperature changes greatly, and is unfavorable for device The stability of part work.
Patent (patent No. 201510243383) by with Ca, Sn to BaTiO3A position and B position carry out displacement simultaneously and change Property, it is thus achieved that high-k and relatively low dielectric loss.Patent (patent No. 201410606390) epoxy resin modification BaTiO3Ceramic powder is combined with PVDF, substantially increases its breakdown field strength.Patent (patent No. 201210150158.8) By at SrTiO3Middle interpolation MgO, brings up to 17.4kV/mm by breakdown field strength, it is thus achieved that 0.36J/cm3Energy storage density.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that one have high energy storage density medium ceramic material and Preparation method.By adding MAS glass dust in BST powder body, improve the shortcoming that the energy storage density of BST pottery is relatively low, made The material obtained has high-k, high breakdown field strength and good temperature stability.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of high energy storage density medium ceramic material, it is to be composited by BST pottery mixed powder and MAS glass dust, MAS glass The consumption of glass powder is the 0.2% ~ 10% of BST pottery mixed powder quality；Described MAS glass dust is consisting of MgO-Al2O3- SiO2；Described BST pottery mixed powder be by x value be in 0.1-0.5 any value Ba1-xSrxTiO3In single-phase powder body Two or more powder body equimolar mixing, ball milling and obtain.
Further, described MAS glass dust is consisting of: MgO 10-18wt%, Al2O325-35wt% and SiO2 50- 58wt%, the mass percent sum of three kinds of components is 100%.
Further, high (>1600 of its dielectric constant of described ceramic material), dielectric loss low (<0.02), breakdown electric field The high (> 18.0kV/mm of intensity), the high (> 2.50J/cm of energy storage density3) and-55-125 DEG C in the range of change in dielectric constant rate- 13.0%-5.0%。
A kind of method preparing high energy storage density medium ceramic material as above, comprises the following steps:
(1) preparation of MAS glass dust:
By MgO, Al2O3And SiO2Powder is ball milling 8-24 hour in deionized water or ethanol, and ball material mass ratio is not less than 1:1, Tinning amount is the 1/2-4/5 of tank volume, rotational speed of ball-mill 100-250 rev/min；Then at 1475-1550 DEG C, it is incubated 4h melt Melt, then pour in deionized water, after shrend, grind the MAS glass dust obtaining 10-50 micron；
(2) preparation of BST pottery mixed powder:
It is the Ba of any value in 0.1-0.5 by x value1-xSrxTiO3Two or more powder body equimolar in single-phase powder body is mixed Close, ball milling 8-24 hour in deionized water or ethanol；Wherein ball material mass ratio is not less than 1:1, and tinning amount is tank volume 1/2-4/5, rotational speed of ball-mill 100-250 rev/min；After being dried by mixed slurry after ball milling, obtain BST pottery mixed powder Body；
(3) preparation of high energy storage density medium ceramic material:
MAS glass dust prepared by step (1), ball in deionized water is added in the BST pottery mixed powder that step (2) prepares Grinding 24 hours mix homogeneously, ball material mass ratio is not less than 1:1, and tinning amount is the 1/2-4/5 of tank volume, rotational speed of ball-mill 100- 250 revs/min；Mixed slurry after ball milling is dried, and obtains the media ceramic powder of high energy storage density；Powder continuously adds 5 ~ 10wt% poly-vinyl alcohol solution, carries out pelletize to powder, is then pressed into disk or square piece；By after potsherd binder removal at air In prior to 850-950 DEG C be incubated 0-2 hour, be then warmed up to 1150 ~ 1300 DEG C sinter 2-8 hour, it is thus achieved that high energy storage density be situated between Ceramics.
More specifically, in step (2), x value is the Ba of any value in 0.1-0.51-xSrxTiO3Single-phase its preparation side of powder body Method is: take the BaCO that purity is more than 99%3、SrCO3And TiO2As raw material, regulate proportioning raw materials, add deionized water ball milling 8 ~ 24 hours, after drying and screening, mixed powder was incubated pre-burning in 2 ~ 10 hours at 1150-1250 DEG C, prepared Ba1-xSrxTiO3Single-phase Powder body.
In step (1), step (2), step (3), ball-milling medium is in zirconia ball, corundum ball or agate ball one Or it is multiple.
The remarkable advantage of the present invention is:
1) the dielectric energy storage material prepared by the present invention is mainly Ba1-xSrxTiO3System solid solution and MAS glass, all materials Without compositions such as environmentally harmful Pb, Bi, Cd in material, environmentally friendly；
2) by having the Ba of different Curie temperature1-xSrxTiO3Single-phase powder body mixes, and improves single component dielectric normal The shortcoming of number temperature stability difference, so that material has relatively low appearance temperature coefficient while keeping high-k；
3) addition in BST ceramic systems of the MAS glass dust not only can reduce sintering temperature, plays energy-conservation effect；And not Ba with x value1-xSrxTiO3Powder body keeps original crystal structure the most as far as possible, preferably reduces dielectric constant to temperature The dependency of change；
4) addition of MAS glass dust significantly improves dielectric material intensity, thus improves energy storage density and the energy storage efficiency of material； And reduce dielectric loss；
5) the high energy storage density dielectric ceramics obtained by the present invention, its DIELECTRIC CONSTANT ε is 1600 ~ 4800, dielectric loss tan δ Less than 0.02, dielectric strength Eb> 18.0kV/mm, the high (> 2.50J/cm of energy storage density3), in the range of-55-125 DEG C, dielectric constant becomes Rate-13.0%-5.0%.
Accompanying drawing explanation
1) Fig. 1 is the XRD spectrum of high energy storage density medium ceramic material typical sample of the present invention；
2) Fig. 2 is the typical ferroelectric hysteresis loop of high energy storage density medium ceramic material of the present invention.
Detailed description of the invention
In order to make content of the present invention easily facilitate understanding, below in conjunction with detailed description of the invention to of the present invention Technical scheme is described further, but the present invention is not limited only to this.
Comparative example 1
The preparation method of a kind of high energy storage density medium ceramic material, concretely comprises the following steps:
(1) Ba1-xSrxTiO3(x=0.1-0.5) synthesis of one-component ceramic powder body
Respectively according to Ba1-xSrxTiO3(x=0.1,0.2,0.3,0.4,0.5) weighs BaCO3、SrCO3、TiO2Powder, weighs Powder ball milling 24 hours in deionized water, wherein ball-milling medium is zirconia ball, and ball material mass ratio is 2:1, and tinning amount is The 1/2 of tank volume, rotational speed of ball-mill 250 revs/min；Mixed slurry after ball milling is dried and is placed in alumina crucible 1150 DEG C Lower pre-burning 2 hours, obtains Ba respectively0.9Sr0.1TiO3、Ba0.8Sr0.2TiO3、Ba0.7Sr0.3TiO3、Ba0.6Sr0.4TiO3、 Ba0.5Sr0.5TiO3These 5 kinds of single-phase powder body；
(2) preparation of BST pottery mixed powder
By the Ba of synthesis in step (1)0.9Sr0.1TiO3、Ba0.8Sr0.2TiO3、Ba0.7Sr0.3TiO3、Ba0.6Sr0.4TiO3With Ba0.5Sr0.5TiO3These 5 kinds of crystalline phases weigh for 1:1:1:1:1 in molar ratio, ball milling 12 hours, wherein ball milling in deionized water Medium is zirconia ball, and ball material mass ratio is 2:1, and tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 200 revs/min；Ball milling After mixed slurry dry；
(3) preparation of BST ceramic body
BST powder body step (2) obtained mixes with binding agent PVAC polyvinylalcohol solution, and adding proportion is 3wt%, at 100MPa Pressure under be pressed into disk；It is incubated 4 hours, it is thus achieved that fine and close BST ceramic material named BST-0 when 1300 DEG C.
The performance of the sample that this comparative example prepares: dielectric constant 8330, dielectric loss 0.055, dielectric strength 13.1kV/ Mm, energy storage density is 6.32J/cm3, energy storage efficiency 58%；Change in dielectric constant rate-48.0%-8.8% in the range of-55-125 DEG C.
Embodiment 1
The preparation method of a kind of high energy storage density medium ceramic material, concretely comprises the following steps:
(1) Ba1-xSrxTiO3(x=0.1-0.5) synthesis of ceramic powder
Respectively according to Ba1-xSrxTiO3(x=0.1,0.2,0.3,0.4,0.5) weighs BaCO3、SrCO3And TiO2Powder, weighs Good powder ball milling 24 hours in deionized water, wherein ball-milling medium is zirconia ball, and ball/material mass ratio is 2:1, tinning amount For the 1/2 of tank volume, rotational speed of ball-mill 250 revs/min；Mixed slurry after ball milling is dried and is placed in alumina crucible 1150 Pre-burning 2 hours at DEG C, it is thus achieved that Ba0.9Sr0.1TiO3、Ba0.8Sr0.2TiO3、Ba0.7Sr0.3TiO3、Ba0.6Sr0.4TiO3With Ba0.5Sr0.5TiO3These 5 kinds of single-phase powder body；
(2) preparation of MAS glass powder
According to 15% MgO, 35% Al2O3、50% SiO2Mass ratio weigh MgO, Al2O3And SiO2, load weighted powder exists Ball milling 24 hours in deionized water, wherein ball-milling medium is zirconia ball, and ball material mass ratio is 2:1, and tinning amount is tank volume 1/2, rotational speed of ball-mill 250 revs/min；At 1550 DEG C, it is incubated 4h melt, then pours in deionized water, grind after shrend and obtain The glass dust of 10-50 micron；
(3) preparation of BST ceramic powder
By the Ba of synthesis in step (1)0.9Sr0.1TiO3、Ba0.8Sr0.2TiO3、Ba0.7Sr0.3TiO3、Ba0.6Sr0.4TiO3With Ba0.5Sr0.5TiO3These 5 kinds of crystalline phases weigh for 1:1:1:1:1 in molar ratio, and add the MAS glass dust of preparation in step (2), The addition of MAS glass dust is the 1wt% of BST ceramic powder quality, the most in deionized water ball milling 24 hours, wherein ball milling Medium is zirconia ball, and ball material mass ratio is 2:1, and tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 150 revs/min；
(4) preparation of BST-1 pottery
Powder body step (3) obtained mixes with binding agent PVAC polyvinylalcohol solution, and adding proportion is 2.5wt%, at 100MPa Pressure under be pressed into disk；To sinter 2 hours in 1250 DEG C in atmosphere after potsherd binder removal, it is thus achieved that fine and close BST-1 pottery；
The performance of the sample that the present embodiment prepares: dielectric constant 4834, dielectric loss 0.007, dielectric strength 18.5kV/mm, storage Can density be 7.32J/cm3, energy storage efficiency 89.5%；Change in dielectric constant rate-12.8%-4.8% in the range of-55-125 DEG C.
Embodiment 2
The preparation method of a kind of high energy storage density medium ceramic material, concretely comprises the following steps:
(1) Ba1-xSrxTiO3(x=0.1-0.5) synthesis of ceramic powder
According to Ba1-xSrxTiO3(x=0.1,0.2,0.3,0.4,0.5) weighs BaCO3、SrCO3And TiO2Powder, load weighted powder Ball milling 24 hours in ethanol, end, wherein ball-milling medium is corundum ball, and ball material mass ratio is 1:1, and tinning amount is tank volume 1/2, rotational speed of ball-mill 250 revs/min；Mixed slurry after ball milling is dried and is placed in alumina crucible 1150 DEG C of pre-burnings 2 hours, Obtain Ba0.9Sr0.1TiO3、Ba0.8Sr0.2TiO3、Ba0.7Sr0.3TiO3、Ba0.6Sr0.4TiO3And Ba0.5Sr0.5TiO3These 5 kinds single-phase Powder body；
(2) preparation of MAS glass powder
According to 13wt% MgO, 32wt% Al2O3、55wt% SiO2Ratio weigh MgO, Al2O3And SiO2, load weighted powder Ball milling 8 hours in ethanol, wherein ball-milling medium is corundum ball, and ball material mass ratio is 1:1, and tinning amount is the 1/2 of tank volume, Rotational speed of ball-mill 250 revs/min；At 1520 DEG C, it is incubated 4h melt, then pours in deionized water, grind after shrend and obtain 10-50 The glass dust of micron；
(3) preparation of BST ceramic powder
By the Ba of synthesis in step (1)0.9Sr0.1TiO3、Ba0.8Sr0.2TiO3、Ba0.7Sr0.3TiO3、Ba0.6Sr0.4TiO3With Ba0.5Sr0.5TiO3These 5 kinds of crystalline phases weigh for 1:1:1:1:1 in molar ratio, and add the MAS glass dust of preparation in step (2), The addition of MAS glass dust is the 2wt% of BST ceramic powder quality, then ball milling 24 hours, wherein ball-milling medium in ethanol For corundum ball, ball material mass ratio is 1:1, and tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 150 revs/min；
(4) preparation of BST-2 pottery
Powder body step (3) obtained mixes with binding agent PVAC polyvinylalcohol solution, and adding proportion is 2.5wt%, at 100MPa Pressure under be pressed into disk；To sinter 2 hours in 1225 DEG C in atmosphere after potsherd binder removal, it is thus achieved that fine and close BST-2 pottery.
The performance of the sample that the present embodiment prepares: dielectric constant 3340, dielectric loss 0.015, dielectric strength 19.0kV/ Mm, energy storage density is 5.34J/cm3, energy storage efficiency 78.0%, change in dielectric constant rate-10.8%-in the range of-55-125 DEG C 4.2%。
Embodiment 3
The preparation method of a kind of high energy storage density medium ceramic material, concretely comprises the following steps:
(1) Ba1-xSrxTiO3(x=0.1-0.5) synthesis of ceramic powder
Respectively according to Ba1-xSrxTiO3(x=0.1,0.2,0.3,0.4,0.5) weighs BaCO3、SrCO3And TiO2Powder, weighs Powder ball milling 24 hours in ethanol, wherein ball-milling medium is agate ball, and ball material mass ratio is 3:1, tinning amount be tank body hold Long-pending 1/2, rotational speed of ball-mill 250 revs/min；Mixed slurry after ball milling is dried and is placed on 1150 DEG C of pre-burnings 2 in alumina crucible Hour, it is thus achieved that Ba0.9Sr0.1TiO3、Ba0.8Sr0.2TiO3、Ba0.7Sr0.3TiO3、Ba0.6Sr0.4TiO3And Ba0.5Sr0.5TiO3These 5 kinds Single-phase powder body；
(2) preparation of MAS glass powder
According to 18wt% MgO, 25wt% Al2O3、57wt% SiO2Ratio weigh MgO, Al2O3、SiO2, load weighted powder exists Ball milling 16 hours in ethanol, wherein ball-milling medium is agate ball, and ball material mass ratio is 3:1, and tinning amount is the 3/5 of tank volume, Rotational speed of ball-mill 200 revs/min；At 1480 DEG C, it is incubated 4h melt, then pours in deionized water, grind after shrend and obtain 10-50 The glass dust of micron；
(3) preparation of BST ceramic powder
By the Ba of synthesis in step (1)0.9Sr0.1TiO3、Ba0.8Sr0.2TiO3、Ba0.7Sr0.3TiO3、Ba0.6Sr0.4TiO3With Ba0.5Sr0.5TiO3These 5 kinds of crystalline phases weigh for 1:1:1:1:1 in molar ratio, and add the MAS glass dust of preparation in step (2), The addition of MAS glass dust is the 5wt% of BST ceramic powder quality, then ball milling 24 hours, wherein ball-milling medium in ethanol For corundum ball, ball material mass ratio is 3:1, and tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 150 revs/min；
(4) preparation of BST-3 pottery
Powder body step (3) obtained mixes with binding agent PVAC polyvinylalcohol solution, and adding proportion is 2.5wt%, at 100MPa Pressure under be pressed into disk；To sinter 2 hours in 1200 DEG C in atmosphere after potsherd binder removal, it is thus achieved that fine and close BST-3 pottery.
The performance of the sample that the present embodiment prepares: dielectric constant 1691, dielectric loss: 0.016, dielectric strength 19.2kV/ Mm, energy storage density is 2.76J/cm3, energy storage efficiency: change in dielectric constant rate-10.5%-in the range of 72.5% ,-55-125 DEG C 4.0%。
Embodiment 4
The preparation method of a kind of high energy storage density medium ceramic material, concretely comprises the following steps:
(1) Ba1-xSrxTiO3(x=0.1-0.5) synthesis of ceramic powder
Respectively according to Ba1-xSrxTiO3(x=0.1,0.15,0.2,0.25,0.3,0.35,0.4,0.45,0.5) weighs BaCO3、 SrCO3And TiO2Powder, load weighted powder is ball milling 24 hours in ethanol, and wherein ball-milling medium is agate ball, ball material mass ratio For 1:1, tinning amount is the 1/2 of tank volume, rotational speed of ball-mill 250 revs/min；Mixed slurry after ball milling is dried and is placed on oxidation 1150 DEG C of pre-burnings 2 hours in aluminum crucible, it is thus achieved that Ba0.9Sr0.1TiO3、Ba0.85Sr0.15TiO3、Ba0.8Sr0.2TiO3、 Ba0.75Sr0.25TiO3、Ba0.7Sr0.3TiO3、Ba0.65Sr0.35TiO3、Ba0.6Sr0.4TiO3、Ba0.55Sr0.55TiO3With Ba0.5Sr0.5TiO3Totally 9 kinds of single-phase BST powder body；
(2) preparation of MAS glass powder
According to 15wt% MgO, 28wt% Al2O3、57wt% SiO2Ratio weigh MgO, Al2O3And SiO2, load weighted powder Ball milling 8 hours in ethanol, wherein ball-milling medium is zirconia ball, and ball material mass ratio is 1:1, and tinning amount is the 1/ of tank volume 2, rotational speed of ball-mill 100 revs/min；At 1500 DEG C, it is incubated 4h melt, then pours in deionized water, grind after shrend and obtain 10- The glass dust of 50 microns；
(3) preparation of BST ceramic powder
By the Ba of synthesis in step (1)0.9Sr0.1TiO3、Ba0.85Sr0.15TiO3、Ba0.8Sr0.2TiO3、Ba0.75Sr0.25TiO3、 Ba0.7Sr0.3TiO3、Ba0.65Sr0.35TiO3、Ba0.6Sr0.4TiO3、Ba0.55Sr0.55TiO3And Ba0.5Sr0.5TiO3Totally 9 kinds single-phase BST powder body weighs according to equimolar, and adds the MAS glass dust of preparation in step (2), and the addition of MAS glass dust is BST pottery The 5wt% of porcelain powder quality, then ball milling 24 hours in ethanol, wherein ball-milling medium is zirconia ball, and ball/material mass ratio is 1:1, tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 150 revs/min；
(4) preparation of BST-4 pottery
Powder body step (3) obtained mixes with binding agent PVAC polyvinylalcohol solution, and adding proportion is 2.5wt%, at 100MPa Pressure under be pressed into square piece；To sinter 2 hours in 1200 DEG C in atmosphere after potsherd binder removal, it is thus achieved that fine and close BST-4 pottery.
The performance of the sample that the present embodiment prepares: dielectric constant 1780, dielectric loss: 0.015, dielectric strength 18.1kV/ Mm, energy storage density is 2.58J/cm3, energy storage efficiency: change in dielectric constant rate-8.9%-in the range of 77.5% ,-55-125 DEG C 4.5%。
Embodiment 5
The preparation method of a kind of high energy storage density medium ceramic material, concretely comprises the following steps:
(1) Ba1-xSrxTiO3(x=0.1-0.5) synthesis of ceramic powder
According to Ba1-xSrxTiO3(x=0.1,0.15,0.2,0.25,0.3,0.35,0.4,0.45,0.5) weighs BaCO3、SrCO3 And TiO2Powder, load weighted powder ball milling 24 hours in deionized water, wherein ball-milling medium is corundum ball, ball material mass ratio For 1:1, tinning amount is the 1/2 of tank volume, rotational speed of ball-mill 250 revs/min；Mixed slurry after ball milling is dried and is placed on oxidation 1200 DEG C of pre-burnings 2 hours in aluminum crucible, it is thus achieved that Ba0.9Sr0.1TiO3、Ba0.85Sr0.15TiO3、Ba0.8Sr0.2TiO3、 Ba0.75Sr0.25TiO3、Ba0.7Sr0.3TiO3、Ba0.65Sr0.35TiO3、Ba0.6Sr0.4TiO3、Ba0.55Sr0.55TiO3With Ba0.5Sr0.5TiO3Totally 9 kinds of single-phase BST powder body；
(2) preparation of MAS glass powder
According to 16% MgO, 32% Al2O3、52% SiO2Ratio weigh MgO, Al2O3And SiO2, load weighted powder go from Ball milling 15 hours in sub-water, wherein ball-milling medium is zirconia ball, and ball material mass ratio is 1:1, and tinning amount is the 4/ of tank volume 5, rotational speed of ball-mill 150 revs/min；At 1525 DEG C, it is incubated 4h melt, then pours in deionized water, grind after shrend and obtain 10- The glass dust of 50 microns；
(3) preparation of BST ceramic powder
By the Ba of synthesis in step (1)0.9Sr0.1TiO3、Ba0.85Sr0.15TiO3、Ba0.8Sr0.2TiO3、Ba0.75Sr0.25TiO3、 Ba0.7Sr0.3TiO3、Ba0.65Sr0.35TiO3、Ba0.6Sr0.4TiO3、Ba0.55Sr0.55TiO3And Ba0.5Sr0.5TiO3Totally 9 kinds single-phase BST powder body weighs according to equimolar, and adds MAS glass dust prepared by step (2), and the addition of MAS glass dust is BST pottery The 5wt% of powder quality, the most in deionized water ball milling 24 hours, wherein ball-milling medium is zirconia ball, and ball material mass ratio is 1:1, tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 150 revs/min；
(4) preparation of BST-5 pottery
Powder body step (3) obtained mixes with binding agent PVAC polyvinylalcohol solution, and adding proportion is 2.5wt%, at 100MPa Pressure under be pressed into disk or square piece；By being incubated 2 hours prior to 950 DEG C in atmosphere after potsherd binder removal, then it is warmed up to 1200 DEG C re-sinter 2 hours, it is thus achieved that fine and close BST-5 pottery.
The performance of the sample that the present embodiment prepares: dielectric constant 1926, dielectric loss 0.008, dielectric strength 25.6kV/ Mm, energy storage density is 5.59J/cm3, energy storage efficiency 82.0%, change in dielectric constant rate-8.2%-4.0% in the range of-55-125 DEG C.
Embodiment 6
The preparation method of a kind of high energy storage density medium ceramic material, concretely comprises the following steps:
(1) Ba1-xSrxTiO3(x=0.1-0.5) synthesis of ceramic powder
According to Ba1-xSrxTiO3(x=0.1,0.15,0.2,0.25,0.3,0.35,0.4,0.45,0.5) weighs BaCO3、SrCO3 And TiO2Powder, load weighted powder ball milling 16 hours in deionized water, wherein ball-milling medium is corundum ball, ball material mass ratio For 1.5:1, tinning amount is the 1/2 of tank volume, rotational speed of ball-mill 250 revs/min；Mixed slurry after ball milling is dried and is placed on oxygen Change in aluminum crucible 1250 DEG C of pre-burnings 2 hours, it is thus achieved that Ba0.9Sr0.1TiO3、Ba0.85Sr0.15TiO3、Ba0.8Sr0.2TiO3、 Ba0.75Sr0.25TiO3、Ba0.7Sr0.3TiO3、Ba0.65Sr0.35TiO3、Ba0.6Sr0.4TiO3、Ba0.55Sr0.55TiO3With Ba0.5Sr0.5TiO3Totally 9 kinds of single-phase BST powder body；
(2) preparation of MAS glass powder
According to 15% MgO, 32% Al2O3、53% SiO2Ratio weigh MgO, Al2O3And SiO2, load weighted powder go from Ball milling 15 hours in sub-water, wherein ball-milling medium is zirconia ball, and ball material mass ratio is 1.5:1, and tinning amount is tank volume 4/5, rotational speed of ball-mill 150 revs/min；At 1520 DEG C, it is incubated 4h melt, then pours in deionized water, grind after shrend and obtain The glass dust of 10-50 micron；
(3) preparation of BST ceramic powder
By the Ba of synthesis in step (1)0.9Sr0.1TiO3、Ba0.85Sr0.15TiO3、Ba0.8Sr0.2TiO3、Ba0.75Sr0.25TiO3、 Ba0.7Sr0.3TiO3、Ba0.65Sr0.35TiO3、Ba0.6Sr0.4TiO3、Ba0.55Sr0.55TiO3And Ba0.5Sr0.5TiO3Totally 9 kinds single-phase BST powder body weighs according to equimolar, and adds MAS glass dust prepared by step (2), and the addition of MAS glass dust is BST pottery The 0.2wt% of powder quality, the most in deionized water ball milling 24 hours, wherein ball-milling medium is zirconia ball, ball material mass ratio For 1.5:1, tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 150 revs/min；
(4) preparation of BST-5 pottery
Powder body step (3) obtained mixes with binding agent PVAC polyvinylalcohol solution, and adding proportion is 2.5wt%, at 100MPa Pressure under be pressed into disk or square piece；Then it is warmed up to 1260 DEG C after potsherd binder removal in atmosphere and is incubated 8 hours, it is thus achieved that cause Close BST-6 pottery.
The performance of the sample that the present embodiment prepares: dielectric constant 5780, dielectric loss 0.035, dielectric strength 16.4kV/ Mm, energy storage density is 6.88J/cm3, energy storage efficiency 78.5%, change in dielectric constant rate-18.8%-in the range of-55-125 DEG C 6.5%。
Embodiment 7
The preparation method of a kind of high energy storage density medium ceramic material, concretely comprises the following steps:
(1) Ba1-xSrxTiO3(x=0.1-0.5) synthesis of ceramic powder
According to Ba1-xSrxTiO3(x=0.1,0.15,0.2,0.25,0.3,0.35,0.4,0.45,0.5) weighs BaCO3、SrCO3 And TiO2Powder, load weighted powder ball milling 20 hours in deionized water, wherein ball-milling medium is corundum ball, ball material mass ratio For 2.5:1, tinning amount is the 1/2 of tank volume, rotational speed of ball-mill 250 revs/min；Mixed slurry after ball milling is dried and is placed on oxygen Change in aluminum crucible 1200 DEG C of pre-burnings 2 hours, it is thus achieved that Ba0.9Sr0.1TiO3、Ba0.85Sr0.15TiO3、Ba0.8Sr0.2TiO3、 Ba0.75Sr0.25TiO3、Ba0.7Sr0.3TiO3、Ba0.65Sr0.35TiO3、Ba0.6Sr0.4TiO3、Ba0.55Sr0.55TiO3With Ba0.5Sr0.5TiO3Totally 9 kinds of single-phase BST powder body；
(2) preparation of MAS glass powder
According to 16% MgO, 30% Al2O3、54% SiO2Ratio weigh MgO, Al2O3And SiO2, load weighted powder go from Ball milling 15 hours in sub-water, wherein ball-milling medium is zirconia ball, and ball material mass ratio is 1.8:1, and tinning amount is tank volume 4/5, rotational speed of ball-mill 150 revs/min；At 1500 DEG C, it is incubated 4h melt, then pours in deionized water, grind after shrend and obtain The glass dust of 10-50 micron；
(3) preparation of BST ceramic powder
By the Ba of synthesis in step (1)0.9Sr0.1TiO3、Ba0.85Sr0.15TiO3、Ba0.8Sr0.2TiO3、Ba0.75Sr0.25TiO3、 Ba0.7Sr0.3TiO3、Ba0.65Sr0.35TiO3、Ba0.6Sr0.4TiO3、Ba0.55Sr0.55TiO3And Ba0.5Sr0.5TiO3Totally 9 kinds single-phase BST powder body weighs according to equimolar, and adds MAS glass dust prepared by step (2), and the addition of MAS glass dust is BST pottery The 10wt% of powder quality, the most in deionized water ball milling 20 hours, wherein ball-milling medium is zirconia ball, ball material mass ratio For 1.8:1, tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 150 revs/min；
(4) preparation of BST-5 pottery
Powder body step (3) obtained mixes with binding agent PVAC polyvinylalcohol solution, and adding proportion is 3.5wt%, at 100MPa Pressure under be pressed into disk or square piece；By being incubated 2 hours prior to 850 DEG C in atmosphere after potsherd binder removal, then it is warmed up to 1150 DEG C are incubated 2 hours again, it is thus achieved that fine and close BST-5 pottery.
The performance of the sample that the present embodiment prepares: dielectric constant 1620, dielectric loss 0.006, dielectric strength 22.8kV/ Mm, energy storage density is 3.73J/cm3, energy storage efficiency 84.0%, change in dielectric constant rate-7.9%-4.2% in the range of-55-125 DEG C.
The energy storage characteristic of table 1 embodiment sample
Pottery of the present invention has perovskite crystal phase structure (as shown in Figure 1)；Ceramic material the most of the present invention has elongated Ferroelectric hysteresis loop, so that it is guaranteed that it has higher energy storage efficiency.And table 1 shows that pottery of the present invention has high-k, low Jie Electrical loss, good dielectric constant temperature stability and the energy storage characteristic of excellence.
The foregoing is only presently preferred embodiments of the present invention, all impartial changes done according to scope of the present invention patent with Modify, all should belong to the covering scope of the present invention.

Claims (6)

1. a high energy storage density medium ceramic material, it is characterised in that: described ceramic material its be by BST pottery mixed powder Body and MAS glass dust are composited, and the consumption of MAS glass dust is the 0.2% ~ 10% of BST pottery mixed powder quality；Described MAS glass dust is consisting of MgO-Al2O3-SiO2；Described BST pottery mixed powder be x value be any value in 0.1-0.5 Ba1-xSrxTiO3In single-phase powder body two or more powder body equimolar mixing, ball milling and obtain.
High energy storage density medium ceramic material the most according to claim 1, it is characterised in that: described MAS glass dust its Consist of: MgO 10-18wt%, Al2O325-35wt% and SiO250-58wt%, the mass percent sum of three kinds of components is 100%。
High energy storage density medium ceramic material the most according to claim 1, it is characterised in that: described medium ceramic material Its dielectric constant>1600, dielectric loss<0.02, breakdown field strength>18.0kV/mm, energy storage density>2.50J/cm3。
4. the method preparing high energy storage density medium ceramic material as described in any one of claim 1-3, its feature exists In: comprise the following steps:
(1) preparation of MAS glass dust:
By MgO, Al2O3And SiO2Powder is ball milling 8-24 hour in deionized water or ethanol, and ball material mass ratio is not less than 1:1, Tinning amount is the 1/2-4/5 of tank volume, rotational speed of ball-mill 100-250 rev/min；Then at 1475-1550 DEG C, it is incubated 4h melt Melt, then pour in deionized water, after shrend, grind the MAS glass dust obtaining 10-50 micron；
(2) preparation of BST pottery mixed powder:
It is the Ba of any value in 0.1-0.5 by x value1-xSrxTiO3Two or more powder body equimolar mixing in single-phase powder body, Ball milling 8-24 hour in deionized water or ethanol；Wherein ball material mass ratio is not less than 1:1, and tinning amount is the 1/ of tank volume 2-4/5, rotational speed of ball-mill 100-250 rev/min；After being dried by mixed slurry after ball milling, obtain BST pottery mixed powder；
(3) preparation of high energy storage density medium ceramic material:
MAS glass dust prepared by step (1), ball in deionized water is added in the BST pottery mixed powder that step (2) prepares Grinding 24 hours so that it is mix homogeneously, ball material mass ratio is not less than 1:1, and tinning amount is the 1/2-4/5 of tank volume, rotational speed of ball-mill 100-250 rev/min；Mixed slurry after ball milling is dried, and obtains the media ceramic powder of high energy storage density；Powder continues Add 5 ~ 10wt% poly-vinyl alcohol solution, powder is carried out pelletize, is then pressed into disk or square piece；By after potsherd binder removal Air is incubated 0-2 hour prior to 850-950 DEG C, is then warmed up to 1150 ~ 1300 DEG C and sinters 2-8 hour, it is thus achieved that high energy storage is close Degree medium ceramic material.
The method of high energy storage density medium ceramic material the most according to claim 4, it is characterised in that: in step (2), x takes Value is the Ba of any value in 0.1-0.51-xSrxTiO3Single-phase powder body its preparation method is: take the BaCO that purity is more than 99%3、 SrCO3And TiO2As raw material, regulating proportioning raw materials, add deionized water ball milling 8 ~ 24 hours, after drying and screening, mixed powder exists It is incubated pre-burning in 2 ~ 10 hours at 1150-1250 DEG C, synthesizes Ba1-xSrxTiO3Single-phase powder body.
The method of high energy storage density medium ceramic material the most according to claim 4, it is characterised in that: step (1), step (2), in step (3) ball-milling medium be in zirconia ball, corundum ball or agate ball one or more.
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