CN106187189A - A kind of energy storage microwave dielectric ceramic materials and preparation method thereof - Google Patents

A kind of energy storage microwave dielectric ceramic materials and preparation method thereof Download PDF

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CN106187189A
CN106187189A CN201610541177.1A CN201610541177A CN106187189A CN 106187189 A CN106187189 A CN 106187189A CN 201610541177 A CN201610541177 A CN 201610541177A CN 106187189 A CN106187189 A CN 106187189A
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郑兴华
刘洋
肖腾
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Fuzhou University
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Abstract

The invention discloses a kind of energy storage microwave dielectric ceramic materials and preparation method thereof.First pre-burned is for CaTiO3‑NdAlO3Powder body, then adds different amounts of MgO Al2O3‑SiO2Glass powder, finally prepares energy storage microwave dielectric ceramic materials.Ceramic material of the present invention has perovskite crystal phase structure and good compactness (relative density > 99%), and there is microwave dielectric property and the energy-storage property of excellence: DIELECTRIC CONSTANT ε is 30 ~ 100, breakdown field strength Eb is 180 ~ 531kV/cm, and energy storage density E is 0.08 ~ 0.5J/cm3, microwave dielectric property (2 ~ 15GHz scope): DIELECTRIC CONSTANT ε is 30 ~ 100, Qf is 15000 20000GHz, temperature coefficient adjustable.Preparation technology of the present invention is simple, and sintering temperature is relatively low, has great industrial application value.

Description

A kind of energy storage microwave dielectric ceramic materials and preparation method thereof
Technical field
The invention belongs to electronic ceramics preparation and applied technical field, be specifically related to a kind of energy storage microwave dielectric ceramic materials And preparation method thereof.
Background technology
Along with the continuous consumption of the energy, the non-renewable problem such as oil, natural gas, people's increasing day by day to energy demand Long, the drawback of energy source in addition, tap a new source of energy for this extremely urgent with the problem of energy storage.Media ceramic is as electric capacity Device receives significant attention because of light, environmental protection, the advantage such as efficiently.At present, the material being developed as energy-accumulating medium mainly has three classes: Battery, ultracapacitor and energy-accumulating medium capacitor.Wherein battery is as the highest device of energy storage density, has and meets miniaturization Requirement, but because it utilizes the redox reaction of material, so having the lowest power density (< 500W/kg), simultaneously to ring Border is very harmful.Ultracapacitor has power density more higher than battery and more higher energy storage density than dielectric capacitor, but Its structure is complicated, voltage is low, leakage current is big, cycle period is short in operation.Dielectric capacitor has storage to be released energy soon, transmits Power is big, combination flexibly, technology maturation, the advantage such as cheap.Owing to the essence of pulse device is in the time by pulse energy It is compressed on yardstick, to obtain the high-peak power output of in very short time (20-100ns), therefore as pulse power The high function pulse power of technical equipment main part, capacitor energy storage compared to mechanical energy energy storage and electrochemical energy storage have with Upper advantage so that it is widely used in pulse power device, and be the core of Pulse Power Techniques.Should for pulse power Energy-accumulating medium require there is high dielectric constant and high breakdown field strength.
At present, the rule changed with external electric field according to dielectric polarization character, energy-accumulating medium material can be divided into three kinds: line Property electrolyte, ferroelectric and antiferroelectric material.Although linear dielectric Constant is relatively low, but it is little with powering up outward The change of field frequencies range and change, can be used under high frequency, and have that response is quick, reversible, repeatedly discharge and recharge, energy storage efficiency close The advantage of 100%.Although ferroelectric material has the highest dielectric constant, but dielectric constant can reduce along with the increase of electric field, and And generally breakdown field strength is the highest, thus energy storage density is the highest.Antiferroelectric has high dielectric constant and high breakdown potential Field intensity, therefore has theoretic high energy storage density.Along with the small integrated of microwave communication industries, multifunction quick Development, develops the ceramics as low-loss microwave medium material of series, CaTiO in recent years3-NdAlO3Microwave-medium ceramics is exactly it Middle Typical Representative, it has medium dielectric constant microwave medium, high quality factor and good frequency-temperature coefficient, is widely used in microwave satellite The communications field.
The energy-accumulating medium of report mostly is ferroelectricity antiferroelectric ceramics, glass ceramics and polymer at present, relevant linear electrolyte Report the fewest, and less as the report of energy storage material about microwave dielectric material.CaTiO3-NdAlO3Micro-as Ku frequency range Ripple media ceramic is widely used in satellite digital TV, has potentiality of high-frequency pulse power device applications simultaneously, at present its There is not been reported for energy-storage property.It is contemplated that keep CaTiO3-NdAlO3While the microwave dielectric property that system's pottery is excellent, By adding glass, reduce its firing temperature, widen firing range, and improve breakdown field strength, thus obtain relatively High energy storage density, microwave-medium multifunctional ceramic material.
Summary of the invention
In order to overcome the complex process of existing energy-storing dielectric ceramic, use frequency deficiency on the low side, the present invention provides a kind of energy storage Microwave dielectric ceramic materials and preparation method thereof.Obtained energy storage microwave dielectric material pottery has the microwave dielectric property of excellence Energy and energy storage characteristic.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of energy storage microwave dielectric ceramic materials, its chemical composition expression formula is:
(1-x)CaTiO3-xNdAlO3+a%(mMgO -nAl2O3-kSiO2)；Wherein, x is molar fraction, 0.1≤x≤0.6；a For CaTiO3-NdAlO3The percentage ratio of quality, 1≤a≤30；M, n, k are mass percent, 15≤m≤20,20≤n≤28,52 ≤k≤60。
Described energy storage microwave dielectric ceramic materials: DIELECTRIC CONSTANT ε is 30 ~ 100, breakdown field strength Eb is 180 ~ 531kV/cm, energy storage density E are 0.08 ~ 0.5J/cm3；Microwave dielectric property (2 ~ 15GHz scope): DIELECTRIC CONSTANT ε is 30 ~ 100, Qf is 15000-20000GHz, temperature coefficient adjustable.
The preparation method of energy storage microwave dielectric ceramic materials as above, specifically includes following steps:
(1) (1-x) CaTiO3-xNdAlO3The preparation of powder body
According to chemical formula (1-x) CaTiO3-xNdAlO3Carrying out dispensing, wherein 0.1≤x≤0.6, x is molar fraction, weighs CaCO3、TiO2、Nd2O3And Al2O3Electron level powder；Load weighted powder is mixing and ball milling 8 ~ 24 in deionized water or ethanol Hour, during wherein ball-milling medium is zirconia ball, corundum ball or agate ball one or more, 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 revs/min；Mixed slurry after ball milling is dried rearmounted With 3 hours synthesis (1-x) CaTiO of 1250 ~ 1350 DEG C of insulations in alumina crucible3-xNdAlO3Powder body；
(2) mMgO-nAl2O3-kSiO2The preparation of glass powder
According to chemical formula mMgO-nAl2O3-kSiO2Carry out dispensing, wherein 15≤m≤20,20≤n≤28,52≤k≤60, m, N, k are mass percent, weigh MgO, Al2O3And SiO2Electron level powder mix homogeneously, be placed in earthenware by the powder body of mix homogeneously In crucible, being incubated 4 hours at 1450 ~ 1600 DEG C, then shrend prepares the glass powder of 10-50 micron；
(3) (1-x) CaTiO3-xNdAlO3+a(mMgO -nAl2O3-kSiO2) ceramic is standby
(1-x) CaTiO that step (1) is prepared3-xNdAlO3Powder body and step (2) prepare 1% ~ 30% mMgO- nAl2O3-kSiO2Glass powder is mixing and ball milling 8 ~ 24 hours in deionized water or ethanol, and wherein ball-milling medium is zirconium oxide In ball, corundum ball or agate ball one or more, ball/material mass ratio is not less than 1:1, tinning amount be tank volume 1/2 ~ 4/5, rotational speed of ball-mill 100-250 rev/min；After mixed slurry after ball milling is dried, the powder body prepared and binding agent PVA or PVB solution mixes, and ratio of binder is 3 ~ 10wt%, is pressed into disk under the pressure of 100MPa；Gained potsherd is arranged In atmosphere in being incubated 1-2 hour prior to 850 ~ 950 DEG C after glue, subsequently at 1-6 hour sintering of 1000 ~ 1300 DEG C of insulations, it is thus achieved that Dense ceramic material.
Sample is processed into that two sides is smooth, thickness is the thin slice of 0.7mm, drapes over one's shoulders silver electrode existing.
The remarkable advantage of the present invention is:
The energy storage microwave dielectric ceramic materials that the present invention provides, the raw material of employing is good for without any infringement human body such as Pb, Bi, Cd Health, the composition of pollution environment, preparation technology is simple, and sintering temperature is relatively low；Have excellence microwave dielectric property and energy-storage property: DIELECTRIC CONSTANT ε is 30 ~ 100, and breakdown field strength Eb is 180 ~ 531kV/cm, and energy storage density E is 0.08 ~ 0.5J/cm3, microwave Dielectric properties (2 ~ 15GHz scope): DIELECTRIC CONSTANT ε is 30 ~ 100, Qf is 15000-20000GHz, temperature coefficient adjustable.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the energy storage microwave dielectric ceramic materials 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.
Embodiment 1
(1) (1-x) CaTiO3-xNdAlO3The preparation of preburning powdered material
According to chemical formula (1-x) CaTiO3-xNdAlO3Carrying out dispensing, wherein x=0.3, x is molar fraction, weighs CaCO3、 TiO2、Nd2O3、Al2O3Electron level powder；Load weighted powder ball milling 24 hours in deionized water, wherein ball-milling medium is oxygen Changing zirconium ball, ball/material mass ratio 1.5:1, tinning amount is the 1/2 of tank volume, rotational speed of ball-mill 100 revs/min；Mixing after ball milling Slurry is dried and is placed in alumina crucible with 3 hours synthesis (1-x) CaTiO of 1300 DEG C of insulations3-xNdAlO3Powder body；
(2) mMgO-nAl2O3-kSiO2The preparation of glass powder
According to chemical formula mMgO-nAl2O3-kSiO2Carrying out dispensing, wherein m=15, n=25, k=60, m, n, k are mass percent, Weigh MgO, Al2O3And SiO2Electron level powder mix homogeneously, be placed in the powder body mixed in crucible, and protects in 1500 DEG C Temperature 4 hours, then shrend prepares the glass powder of 10 ~ 50 microns；
(3) (1-x) CaTiO3-xNdAlO3+a(mMgO -nAl2O3-kSiO2) ceramic is standby
By (1-x) CaTiO3-xNdAlO3(x=0.3) ceramic powder and the mMgO-nAl of 2%2O3-kSiO2Glass is at deionized water Middle mixing and ball milling 12 hours, wherein ball-milling medium is zirconia ball, ball/material mass ratio 1.5:1, and tinning amount is the 1/ of tank volume 2, rotational speed of ball-mill 100 revs/min；Mixed slurry after ball milling mixes with binding agent polyvinyl alcohol (PVA) solution after drying, PVA Adding proportion is 8wt%, is pressed into disk under the pressure of 100MPa；Sinter in atmosphere, with stove after gained potsherd binder removal Being warmed up to 950 DEG C and be incubated 1 hour, be then warmed up to 1250 DEG C and be incubated 3 hours, then furnace cooling is to room temperature, it is thus achieved that fine and close Ceramic material.
Sample is processed into that two sides is smooth, thickness is the thin slice of 0.7mm, drapes over one's shoulders silver electrode existing, then tests dielectric properties, meter Calculate energy storage density, performance such as table 1.Sheet test microwave dielectric property (table 2) of another processing 4mm.
Embodiment 2
(1) (1-x) CaTiO3-xNdAlO3The preparation of preburning powdered material
According to chemical formula (1-x) CaTiO3-xNdAlO3Carrying out dispensing, wherein x=0.3, x is molar fraction, weighs CaCO3、 TiO2、Nd2O3、Al2O3Electron level powder；Load weighted powder ball milling 8 hours in deionized water, wherein ball-milling medium is corundum Ball, ball/material mass ratio 2:1, tinning amount is the 3/5 of tank volume, rotational speed of ball-mill 250 revs/min；Mixed slurry after ball milling dries Dry being placed in alumina crucible synthesizes (1-x) CaTiO in 3 hours with 1250 DEG C of insulations3-xNdAlO3Powder body；
(2) mMgO-nAl2O3-kSiO2The preparation of glass powder
According to chemical formula mMgO-nAl2O3-kSiO2Carrying out dispensing, wherein m=20, n=20, k=60, m, n, k are mass percent, Weigh MgO, Al2O3And SiO2Electron level powder mix homogeneously, be placed in the powder body mixed in crucible, and protects in 1470 DEG C Temperature 4 hours, then shrend prepares the glass powder of 10 ~ 50 microns；
(3) (1-x) CaTiO3-xNdAlO3+a(mMgO -nAl2O3-kSiO2) ceramic is standby
By (1-x) CaTiO after preheating3-xNdAlO3Pottery pre-burning powder body and the mMgO-nAl of 5%2O3-kSiO2Glass Ball milling 12 hours in deionized water, wherein ball-milling medium is corundum ball, ball/material mass ratio 2:1, and tinning amount is tank volume 3/5, rotational speed of ball-mill 250 revs/min；After mixed slurry after ball milling is dried, the powder body prepared and binding agent polyvinyl alcohol (PVA) Solution mixes, and PVA adding proportion is 8wt%, is pressed into disk under the pressure of 100MPa；By after prepared potsherd binder removal Sintering in air, be warmed up to 850 DEG C with stove and be incubated 2 hours, be then warmed up to 1200 DEG C and be incubated 6 hours, then furnace cooling arrives Room temperature, it is thus achieved that fine and close ceramic material.
Sample is processed into that two sides is smooth, thickness is the thin slice of 0.7mm, drapes over one's shoulders silver electrode existing, then tests dielectric properties, meter Calculate energy storage density, performance such as table 1.Sheet test microwave dielectric property (table 2) of another processing 4mm.
Embodiment 3
(1) (1-x) CaTiO3-xNdAlO3The preparation of preburning powdered material
According to chemical formula (1-x) CaTiO3-xNdAlO3Carrying out dispensing, wherein x=0.3, x is molar fraction, weighs CaCO3、 TiO2、Nd2O3、Al2O3Electron level powder；Load weighted powder is ball milling 16 hours in ethanol, and wherein ball-milling medium is agate ball, Ball/material mass ratio 2.1:1, tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 200 revs/min；Mixed slurry after ball milling dries Dry being placed in alumina crucible synthesizes (1-x) CaTiO in 3 hours with 1300 DEG C of insulations3-xNdAlO3Powder body；
(2) mMgO-nAl2O3-kSiO2The preparation of glass powder
According to chemical formula mMgO-nAl2O3-kSiO2Carrying out dispensing, wherein m=18, n=28, k=54, m, n, k are mass percent, Weigh MgO, Al2O3And SiO2Electron level powder mix homogeneously, be placed in the powder body mixed in crucible, and protects in 1550 DEG C Temperature 4 hours, then shrend prepares the glass powder of 10 ~ 50 microns；
(3) (1-x) CaTiO3-xNdAlO3+a(mMgO -nAl2O3-kSiO2) ceramic is standby
By (1-x) CaTiO after preheating3-xNdAlO3Pottery pre-burning powder body and the mMgO-nAl of 10%2O3-kSiO2Glass Ball milling 8 hours in ethanol, wherein ball-milling medium is zirconia ball and corundum ball, ball/material mass ratio 2.1:1, and tinning amount is tank The 1/2 of body volume, rotational speed of ball-mill 150 revs/min；After mixed slurry after ball milling is dried, the powder body prepared and the poly-second of binding agent Enol (PVA) solution mixes, and PVA adding proportion is 3wt%, is pressed into disk under the pressure of 100MPa；Gained potsherd is arranged Sinter in atmosphere after glue, with stove be warmed up to 900 DEG C be incubated 1.5 hours, be then warmed up to 1150 DEG C be incubated 2 hours, then with Stove is cooled to room temperature, it is thus achieved that fine and close ceramic material.
Sample is processed into that two sides is smooth, thickness is the thin slice of 0.7mm, drapes over one's shoulders silver electrode existing, then tests dielectric properties, meter Calculate energy storage density, performance such as table 1.Sheet test microwave dielectric property (table 2) of another processing 4mm.
Embodiment 4
(1) (1-x) CaTiO3-xNdAlO3The preparation of preburning powdered material
According to chemical formula (1-x) CaTiO3-xNdAlO3Carrying out dispensing, wherein x=0.3, x is molar fraction, weighs CaCO3、 TiO2、Nd2O3、Al2O3Electron level powder；Load weighted powder ball milling 12 hours in deionized water, wherein ball-milling medium is firm Beautiful ball and agate ball, ball/material mass ratio 2.2:1, tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 200 revs/min；After ball milling Mixed slurry dry be placed in alumina crucible with 1300 DEG C insulation 3 hours synthesis (1-x) CaTiO3-xNdAlO3Pre-burning powder Body；
(2) mMgO-nAl2O3-kSiO2The preparation of glass powder
According to chemical formula mMgO-nAl2O3-kSiO2Carrying out dispensing, wherein m=20, n=28, k=52, m, n, k are mass percent, Weigh MgO, Al2O3And SiO2Electron level powder mix homogeneously, be placed in the powder body mixed in crucible, and protects in 1550 DEG C Temperature 4 hours, then shrend prepares the glass powder of 10 ~ 50 microns；
(3) (1-x) CaTiO3-xNdAlO3+a(mMgO -nAl2O3-kSiO2) ceramic is standby
By (1-x) CaTiO after preheating3-xNdAlO3(x=0.3) pottery pre-burning powder body and the mMgO-nAl of 20%2O3- kSiO2Glass ball milling 12 hours in deionized water, wherein ball-milling medium is corundum ball and agate ball, ball/material mass ratio 2.2: 1, tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 150 revs/min；After mixed slurry after ball milling is dried, the powder body prepared Mixing with binding agent polyvinyl alcohol (PVA) solution, PVA adding proportion is 10wt%, is pressed into disk under the pressure of 100MPa； Sinter in atmosphere after prepared potsherd binder removal, be warmed up to 850 DEG C with stove and be incubated 2 hours, be then warmed up to 1100 DEG C of guarantors Temperature 2 hours, then furnace cooling is to room temperature, it is thus achieved that fine and close ceramic material；
Sample is processed into that two sides is smooth, thickness is the thin slice of 0.7mm, drapes over one's shoulders silver electrode existing, then tests dielectric properties, calculates storage Energy density, performance such as table 1.Sheet test microwave dielectric property (table 2) of another processing 4mm.
Embodiment 5
(1) (1-x) CaTiO3-xNdAlO3The preparation of preburning powdered material
According to chemical formula (1-x) CaTiO3-xNdAlO3Carrying out dispensing, wherein x=0.2, x is molar fraction, weighs CaCO3、 TiO2、Nd2O3、Al2O3Electron level powder；Load weighted powder is ball milling 18 hours in ethanol, and wherein ball-milling medium is zirconium oxide Ball, ball/material mass ratio 2.3:1, tinning amount is the 1/2 of tank volume, rotational speed of ball-mill 250 revs/min；Mixed slurry after ball milling Drying is placed in alumina crucible with 3 hours synthesis (1-x) CaTiO of 1300 DEG C of insulations3-xNdAlO3Pre-burning powder body；
(2) mMgO-nAl2O3-kSiO2The preparation of glass powder
According to chemical formula mMgO-nAl2O3-kSiO2Carrying out dispensing, wherein m=20, n=25, k=55, m, n, k are mass percent, Weigh MgO, Al2O3And SiO2Electron level powder mix homogeneously, be placed in the powder body mixed in crucible, and protects in 1500 DEG C Temperature 4 hours, then shrend prepares the glass powder of 10 ~ 50 microns；
(3) (1-x) CaTiO3-xNdAlO3+a(mMgO -nAl2O3-kSiO2) ceramic is standby
By (1-x) CaTiO after preheating3-xNdAlO3(x=0.2) pottery pre-burning powder body and the mMgO-nAl of 1%2O3- kSiO2Glass ball milling 8 hours in deionized water, wherein ball-milling medium is zirconia ball, ball/material mass ratio 2.3:1, tinning amount For the 3/5 of tank volume, rotational speed of ball-mill 200 revs/min；After mixed slurry after ball milling is dried, the powder body prepared and binding agent Polyvinyl alcohol (PVA) solution mixes, and PVA adding proportion is 5wt%, is pressed into disk under the pressure of 100MPa；By prepared pottery Sinter in atmosphere after ceramics binder removal, be warmed up to 950 DEG C with stove and be incubated 1 hour, be then warmed up to 1300 DEG C and be incubated 1 hour, so Rear furnace cooling is to room temperature, it is thus achieved that fine and close ceramic material；
Sample is processed into that two sides is smooth, thickness is the thin slice of 0.7mm, drapes over one's shoulders silver electrode existing, then tests dielectric properties, calculates storage Energy density, performance such as table 1.Sheet test microwave dielectric property (table 2) of another processing 4mm.
Embodiment 6
(1) (1-x) CaTiO3-xNdAlO3The preparation of preburning powdered material
According to chemical formula (1-x) CaTiO3-xNdAlO3Carrying out dispensing, wherein x=0.4, x is molar fraction, weighs CaCO3、 TiO2、Nd2O3、Al2O3Electron level powder；Load weighted powder ball milling 24 hours in deionized water, wherein ball-milling medium is firm Beautiful ball, ball/material mass ratio 2.5:1, tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 200 revs/min；Mixing slurry after ball milling Material drying is placed in alumina crucible with 3 hours synthesis (1-x) CaTiO of 1300 DEG C of insulations3-xNdAlO3Pre-burning powder body；
(2) mMgO-nAl2O3-kSiO2The preparation of glass powder
According to chemical formula mMgO-nAl2O3-kSiO2Carrying out dispensing, wherein m=20, n=26, k=54, m, n, k are mass percent, Weigh MgO, Al2O3And SiO2Electron level powder mix homogeneously, be placed in the powder body mixed in crucible, and protects in 1570 DEG C Temperature 4 hours, then shrend prepares the glass powder of 10 ~ 50 microns；
(3) (1-x) CaTiO3-xNdAlO3+a(mMgO -nAl2O3-kSiO2) ceramic is standby
By (1-x) CaTiO after preheating3-xNdAlO3(x=0.4) pottery pre-burning powder body and the mMgO-nAl of 30%2O3- kSiO2Glass is ball milling 8 hours in ethanol, and wherein ball-milling medium is corundum ball, ball/material mass ratio 2.5:1, and tinning amount is tank body The 4/5 of volume, rotational speed of ball-mill 200 revs/min；After mixed slurry after ball milling is dried, the powder body prepared and binding agent PVB solution Mixing, PVB adding proportion is 8wt%, is pressed into disk under the pressure of 100MPa；Sinter in atmosphere after potsherd binder removal, Being warmed up to 950 DEG C with stove and be incubated 1 hour, be then warmed up to 1000 DEG C and be incubated 2 hours, then furnace cooling is to room temperature, it is thus achieved that cause Close ceramic material；
Sample is processed into that two sides is smooth, thickness is the thin slice of 0.7mm, drapes over one's shoulders silver electrode existing, then tests dielectric properties, calculates storage Energy density, performance such as table 1.Sheet test microwave dielectric property (table 2) of another processing 4mm.
Embodiment 7
(1) (1-x) CaTiO3-xNdAlO3The preparation of preburning powdered material
According to chemical formula (1-x) CaTiO3-xNdAlO3Carrying out dispensing, wherein x=0.1, x is molar fraction, weighs CaCO3、 TiO2、Nd2O3、Al2O3Electron level powder；Load weighted powder ball milling 24 hours in deionized water, wherein ball-milling medium is firm Beautiful ball, ball/material mass ratio 2.5:1, tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 200 revs/min；Mixing slurry after ball milling Material drying is placed in alumina crucible with 3 hours synthesis (1-x) CaTiO of 1300 DEG C of insulations3-xNdAlO3Pre-burning powder body；
(2) mMgO-nAl2O3-kSiO2The preparation of glass powder
According to chemical formula mMgO-nAl2O3-kSiO2Carrying out dispensing, wherein m=20, n=26, k=54, m, n, k are mass percent, Weigh MgO, Al2O3And SiO2Electron level powder mix homogeneously, be placed in the powder body mixed in crucible, and protects in 1450 DEG C Temperature 4 hours, then shrend prepares the glass powder of 10 ~ 50 microns；
(3) (1-x) CaTiO3-xNdAlO3+a(mMgO -nAl2O3-kSiO2) ceramic is standby
By (1-x) CaTiO after preheating3-xNdAlO3(x=0.4) pottery pre-burning powder body and the mMgO-nAl of 15%2O3- kSiO2Glass is ball milling 8 hours in ethanol, and wherein ball-milling medium is corundum ball, ball/material mass ratio 2.5:1, and tinning amount is tank body The 4/5 of volume, rotational speed of ball-mill 200 revs/min；After mixed slurry after ball milling is dried, the powder body prepared and binding agent PVB solution Mixing, PVB adding proportion is 8wt%, is pressed into disk under the pressure of 100MPa；Sinter in atmosphere after potsherd binder removal, Being warmed up to 950 DEG C with stove and be incubated 1 hour, be then warmed up to 1150 DEG C and be incubated 2 hours, then furnace cooling is to room temperature, it is thus achieved that cause Close ceramic material.
Embodiment 8
(1) (1-x) CaTiO3-xNdAlO3The preparation of preburning powdered material
According to chemical formula (1-x) CaTiO3-xNdAlO3Carrying out dispensing, wherein x=0.6, x is molar fraction, weighs CaCO3、 TiO2、Nd2O3、Al2O3Electron level powder；Load weighted powder ball milling 24 hours in deionized water, wherein ball-milling medium is firm Beautiful ball, ball/material mass ratio 2.5:1, tinning amount is the 4/5 of tank volume, rotational speed of ball-mill 200 revs/min；Mixing slurry after ball milling Material drying is placed in alumina crucible with 3 hours synthesis (1-x) CaTiO of 1300 DEG C of insulations3-xNdAlO3Pre-burning powder body；
(2) mMgO-nAl2O3-kSiO2The preparation of glass powder
According to chemical formula mMgO-nAl2O3-kSiO2Carrying out dispensing, wherein m=20, n=26, k=54, m, n, k are mass percent, Weigh MgO, Al2O3And SiO2Electron level powder mix homogeneously, be placed in the powder body mixed in crucible, and protects in 1600 DEG C Temperature 4 hours, then shrend prepares the glass powder of 10 ~ 50 microns；
(3) (1-x) CaTiO3-xNdAlO3+a(mMgO -nAl2O3-kSiO2) ceramic is standby
By (1-x) CaTiO after preheating3-xNdAlO3(x=0.4) pottery pre-burning powder body and the mMgO-nAl of 15%2O3- kSiO2Glass is ball milling 8 hours in ethanol, and wherein ball-milling medium is corundum ball, ball/material mass ratio 2.5:1, and tinning amount is tank body The 4/5 of volume, rotational speed of ball-mill 200 revs/min；After mixed slurry after ball milling is dried, the powder body prepared and binding agent PVB solution Mixing, PVB adding proportion is 8wt%, is pressed into disk under the pressure of 100MPa；Sinter in atmosphere after potsherd binder removal, Being warmed up to 950 DEG C with stove and be incubated 1 hour, be then warmed up to 1200 DEG C and be incubated 2 hours, then furnace cooling is to room temperature, it is thus achieved that cause Close ceramic material.
The energy storage characteristic of table 1 embodiment sample
The microwave dielectric property of table 2 embodiment sample
Pottery of the present invention has perovskite crystal phase structure, and is scanned by knowable to Electronic Speculum SEM figure (Fig. 1) having good densification Property (relative density > 99%).By table 1 and 2 understand pottery of the present invention have have under Ku frequency range microwave frequency high-k, High quality factor and nearly zero-temperature coefficient, have good energy storage characteristic simultaneously.
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 (4)

1. an energy storage microwave dielectric ceramic materials, it is characterised in that: the chemical composition expression formula of described ceramic material is: (1- x)CaTiO3-xNdAlO3+a%(mMgO -nAl2O3-kSiO2)；Wherein, x is molar fraction, 0.1≤x≤0.6；A is CaTiO3- NdAlO3The percentage ratio of quality, 1≤a≤30；M, n, k are mass percent, 15≤m≤20,20≤n≤28,52≤k≤60.
Energy storage microwave dielectric ceramic materials the most according to claim 1, it is characterised in that: described energy storage microwave-medium ceramics The DIELECTRIC CONSTANT ε of material is 30 ~ 100, and Qf is 15000-20000GHz, and breakdown field strength Eb is 180 ~ 531kV/cm, energy storage Density E is 0.08 ~ 0.5J/cm3。
3. the preparation method of the energy storage microwave dielectric ceramic materials as described in claim 1-2, it is characterised in that: concrete Comprise the following steps:
(1) (1-x) CaTiO3-xNdAlO3The preparation of powder body
According to chemical formula (1-x) CaTiO3-xNdAlO3Carry out dispensing, weigh CaCO3、TiO2、Nd2O3And Al2O3Electron level powder； Load weighted powder is mixing and ball milling 8 ~ 24 hours in deionized water or ethanol；Mixed slurry after ball milling is dried and is placed on oxygen Change in aluminum crucible with 3 hours synthesis (1-x) CaTiO of 1250 ~ 1350 DEG C of insulations3-xNdAlO3Powder body；
(2) mMgO-nAl2O3-kSiO2The preparation of glass powder
According to chemical formula mMgO-nAl2O3-kSiO2Carry out dispensing, weigh MgO, Al2O3And SiO2Electron level powder also mixes all Even, the powder body of mix homogeneously is placed in crucible, in 1450 ~ 1600 DEG C, is incubated 4 hours, then shrend prepares 10-50 micron Glass powder；
(3) (1-x) CaTiO3-xNdAlO3 +a(mMgO -nAl2O3-kSiO2) ceramic is standby
(1-x) CaTiO that step (1) is prepared3-xNdAlO3MMgO-the nAl that powder body prepares with step (2)2O3-kSiO2Glass Powder body is mixing and ball milling 8-24 hour in deionized water or ethanol；After mixed slurry after ball milling is dried, the powder body prepared with Binding agent PVA or the mixing of PVB solution, ratio of binder is 3 ~ 10wt%, is pressed into disk under the pressure of 100MPa； By after gained potsherd binder removal in atmosphere in prior to 850 ~ 950 DEG C be incubated 1 ~ 2 hour, subsequently 1000 ~ 1300 DEG C be incubated 1 ~ 6 Hour sintering, it is thus achieved that dense ceramic material.
The preparation method of a kind of energy storage microwave dielectric ceramic materials the most according to claim 3, it is characterised in that: step (1) technological parameter of ball milling is and in step (3): ball-milling medium be a kind of in zirconia ball, corundum ball or agate ball or Multiple, 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.
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CN111825445A (en) * 2019-04-22 2020-10-27 中南大学深圳研究院 High-dielectric-constant microwave dielectric ceramic material, preparation and application thereof
CN111825445B (en) * 2019-04-22 2023-02-17 中南大学深圳研究院 High-dielectric-constant microwave dielectric ceramic material, preparation and application thereof
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CN112876239A (en) * 2021-03-15 2021-06-01 无锡市高宇晟新材料科技有限公司 Cordierite-doped complex-phase microwave dielectric ceramic material, preparation method and application thereof
CN115838283A (en) * 2022-12-19 2023-03-24 华南理工大学 Energy storage composite material and preparation method thereof
CN115838283B (en) * 2022-12-19 2023-12-15 华南理工大学 Energy storage composite material and preparation method thereof

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