CN110204335A - Ceramic material and preparation method thereof a kind of while that there is high energy storage density and efficiency - Google Patents
Ceramic material and preparation method thereof a kind of while that there is high energy storage density and efficiency Download PDFInfo
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- 238000004146 energy storage Methods 0.000 title claims abstract description 53
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000005498 polishing Methods 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000000498 ball milling Methods 0.000 claims abstract description 27
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052709 silver Inorganic materials 0.000 claims abstract description 25
- 239000004332 silver Substances 0.000 claims abstract description 25
- 239000000126 substance Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 75
- 239000000843 powder Substances 0.000 claims description 67
- 239000000919 ceramic Substances 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 28
- 238000010792 warming Methods 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 27
- 235000019441 ethanol Nutrition 0.000 claims description 27
- 238000001816 cooling Methods 0.000 claims description 21
- 235000015895 biscuits Nutrition 0.000 claims description 20
- 238000004321 preservation Methods 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 11
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 7
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 7
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 7
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 7
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 7
- 230000008595 infiltration Effects 0.000 claims description 7
- 238000001764 infiltration Methods 0.000 claims description 7
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 7
- 239000003973 paint Substances 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 5
- 239000012459 cleaning agent Substances 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 238000012956 testing procedure Methods 0.000 claims description 2
- 125000003636 chemical group Chemical group 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 6
- 239000004615 ingredient Substances 0.000 abstract description 2
- 239000011734 sodium Substances 0.000 description 30
- 239000003990 capacitor Substances 0.000 description 8
- 230000010287 polarization Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 230000015556 catabolic process Effects 0.000 description 6
- 238000007873 sieving Methods 0.000 description 6
- 238000011056 performance test Methods 0.000 description 5
- 229910003378 NaNbO3 Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002241 glass-ceramic Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000005553 drilling Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 230000008450 motivation Effects 0.000 description 1
- 230000005658 nuclear physics Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 210000002381 plasma Anatomy 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- UYLYBEXRJGPQSH-UHFFFAOYSA-N sodium;oxido(dioxo)niobium Chemical compound [Na+].[O-][Nb](=O)=O UYLYBEXRJGPQSH-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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Abstract
The invention discloses a kind of ceramic material and preparation method thereof simultaneously with high energy storage density and efficiency, chemical formula is (1-x) NaNbO3‑x(Bi0.5Na0.5)HfO3, wherein 0.05≤x≤0.2；The material by ingredient, ball milling, pre-burning, secondary ball milling, granulating and forming, dumping, obtained at burning, polishing and by silver electrode.Energy storage density based on ferroelectric hysteresis loop calculating is in 0.99~3.51J/cm3Between, energy storage efficiency is between 60~80.1%.The material has energy storage density high as a kind of novel energy storage ceramic material, and preparation process is simple, at low cost, pollution-free, is easy to the advantages that being mass produced, has strong practicability.
Description
Technical field
The present invention relates to dielectric energy storage ceramic field of material technology, and in particular to it is a kind of have simultaneously high energy storage density and
Sodium niobate base ceramic material of high energy storage efficiency and preparation method thereof.
Background technique
Later period the 1970s, with technologies such as nuclear physics, electron beam, accelerator, laser, electric discharge theory and plasmas
Research and increasingly extensive application, Pulse Power Techniques start to be widely used in national defence, scientific experiment, industrial or agricultural and medicine neck
In domain.Since the 21th century, Pulse Power Techniques and high voltage new technology are increasingly becoming current subject coverage and high-tech
The very high new branch of science of integrated level is one of most great-hearted subdiscipline in Electrotechnics field.With the hair of science and technology
Exhibition, especially needs of the developed country in national defence and space programme, Pulse Power Techniques are gradually paid attention to.Pulse power skill
Art refers to the primary pulse waveform (millisecond to delicate) needed for being generated by initial energy storage technology, then recycles pulse shaping and opens
Pass technology is compressed in time scale by the pulse to energy, shaping, realizes the amplification of output pulse peak power,
And it is output to load, high intensity pulsing electromagnetic field power source is provided for high-tech device and new concept weapon.The main body of pulse power device is
High power pulsed source provides electromagnetic energy for the load of pulse power device.Generally, Pulse Power Techniques include initial energy
Source, intermediate energy storage, pulse compression and several links such as transformation and load.
Currently, the type of Initial energy source mainly has electric energy (solid-state capacitor, supercapacitor, inductance etc.), mechanical energy (electricity
Motivation, inertia energy storage) and chemical energy (lithium battery, fuel cell).Wherein solid-state capacitor with its high power density (~
108W/kg), fast charge/discharge speed (nanosecond to microsecond) and to become Pulse Power Techniques long cycle life (~50 ten thousand times) excellent
The energy storage mode first selected, but its energy storage density (Wrec) relatively low (10-2-10-1Wh/kg), it is not able to satisfy pulse power device
Part is integrated, lightweight and miniaturization demand.The capacitor applied in great power pulse power source at present is foil structure mostly
Capacitor and metallization film capacitor.The former there are energy storage densities low, the problems such as exploding of easily breaking down；The latter, which exists, uses the longevity
Order short, the deficiencies of discharge current is small.Therefore, for meet needed in great power pulse power source energy-storage travelling wave tube have high energy storage density,
The requirement of the properties such as long charge discharge life and big output electric current, designing and preparing high performance energy-accumulating medium material has
Significance.
Dielectric material currently used for solid-state capacitor mainly include polymer, Ceramic-polymer Composite, glass,
Glass ceramics and ceramic five major class.Relative to other energy-accumulating medium materials, dielectric ceramic has medium disruptive field intensity (Eb), compared with
Low dielectric loss (tan δ), excellent temperature stability and fatigue resistance can better meet aerospace, petroleum drilling
Demand of the fields such as well, electromagnetic pulse weapon to energy-storage capacitor.Thus, ceramic medium material is considered as that preparation high temperature resistant is solid
The excellent material of state capacitor.Current unleaded energy storage ceramic material is concentrated mainly on BaTiO3、SrTiO3、(Bi0.5Na0.5)TiO3、
(K0.5Na0.5)NbO3And AgNbO3On equal ceramic materials, still, these materials are difficult have high energy storage density and high energy storage simultaneously
Efficiency.Such as Shen et al. is prepared for 0.91BaTiO3-0.09BiYbO3Ceramics, energy storage efficiency are up to 87%, but energy storage density
Only 0.71J/cm3；Zhao et al. is prepared for AgNbO3+ 0.1wt%MnO2Ceramics, energy storage density are up to 2.5J/cm3, but store up
Energy efficiency is only 56%, and which has limited their practical applications.Therefore, it designs and prepares and is provided simultaneously with high energy storage density and high storage
The unleaded energy-storing dielectric ceramic of energy efficiency is the technological difficulties that dielectric energy storage ceramic technical field faces at present.
Summary of the invention
In view of the above problems, the present invention is intended to provide a kind of ceramic material simultaneously with high energy storage density and efficiency
Material and preparation method thereof, passes through doping (Bi0.5Na0.5)HfO3In NaNbO3Induced synthesis polar nano microcell in ceramics obtains low
Remanent polarization；High saturated polarization is obtained using the hybridism of the 2p track of the 6s and O of Bi；In addition,
(Bi0.5Na0.5)HfO3Incorporation NaNbO can be significantly reduced3The dielectric loss of base ceramics, improves its consistency, reduces its crystal grain
Size, and then its breakdown strength is improved, it is finally obtained while having the ceramic material of high energy storage density and high energy storage efficiency.
To achieve the goals above, the technical solution adopted in the present invention is as follows:
Ceramic material that is a kind of while having high energy storage density and efficiency, the chemical composition of the ceramic material are (1-x)
NaNbO3-x(Bi0.5Na0.5)HfO3, wherein 0.05≤x≤0.2.
For energy-accumulating medium material, to obtain high energy storage density and energy storage efficiency, it is necessary to have following characteristics: high
Saturated polarization, low remanent polarization and high breakdown strength.
Introduced (the Bi of the present invention0.5Na0.5)HfO3Have the advantage that
(1)(Bi0.5Na0.5)HfO3The 2p orbital hybridization of the 6s and O of middle Bi help to obtain high saturated polarization.
(2) as introducing (Bi0.5Na0.5)HfO3When, (Bi0.5Na0.5)2+And Hf4+Respectively enter NaNbO3The position A of ceramics and B
Its long range ordered structure is broken in position, promotes the formation of polar nano microcell, help to obtain low remanent polarization.
(3)Hf4+Relative to Ti of the same clan4+, there is better chemical stability, advantageously reduce dielectric loss and electric leakage
Stream, and then obtain higher breakdown strength.
(4)(Bi0.5Na0.5)HfO3Introducing can promote NaNbO3The sintering of ceramics, significantly reduces its air vent content and crystalline substance
Particle size, and then obtain high breakdown strength.
A kind of preparation method of ceramic material while that there is high energy storage density and efficiency, comprising the following steps:
S1, weighing is calculated: by analytically pure natrium carbonicum calcinatum, niobium pentaoxide, bismuth oxide and hafnium oxide raw material
Under the conditions of 120-150 DEG C after drying and processing 10-15 hours, by chemical general formula (1-x) NaNbO3-x(Bi0.5Na0.5)HfO3,
Stoichiometric ratio in (0.05≤x≤0.2) successively weighs above-mentioned each raw material, and successively pours into ball grinder, obtains mixture；
S2, ball milling: by the resulting mixture of step S1 in ethanol with ZrO2Ball is medium planetary ball mill 12-20 hours,
Drying sieving, obtains dry powder；The ratio of ethyl alcohol and mixture is 2:1；
S3, pre-burning: the resulting dry powder of step S2 after pre-burning 5-12 hours, is ground up, sieved, is obtained in 870-920 DEG C of air
Powder A；
S4, multiple ball milling: by the resulting powder A of step S3 planetary ball mill 12-20 hours in ethanol, after drying, by powder
Material in ethanol planetary ball mill 12-20 hour again, multiple ball milling is successively carried out, after finally drying, obtains powder material B；
Ethyl alcohol and the ratio of powder A are 2:1, this ratio can make ethyl alcohol just submerge powder just, make the powder of ball milling
It is more uniform, the effect of ball milling can be improved；
S5, granulating and forming: polyvinyl alcohol is added by the 5% of powder quality in the resulting powder material B of step S4 and is granulated, must be shaped
Biscuit；
S6, dumping: the resulting forming biscuit of step S5 being placed in moderate oven and is warming up to 500-650 DEG C, keeps the temperature 2-5 hours
Afterwards, with furnace natural cooling；
S7, at burning: the resulting forming biscuit of step S6 is gradually heated to 1230-1310 DEG C using two step temperature-raising methods, is protected
After 1-5 hours warm, with furnace natural cooling, ceramic of compact piece is obtained.3, one kind according to claim 2 has high storage simultaneously
The preparation method of the ceramic material of energy density and efficiency, which is characterized in that the powder after being granulated in the step S5 is in 100-
It is dry-pressing formed under the pressure of 300MPa.
Preferably, the rate that temperature rises in the step S6 is specially 1-3 DEG C/min.
Preferably, two step temperature-raising methods in the step S7, which refer to, is warming up to 600 with the heating rate of 3-5 DEG C/min
DEG C, then 1230-1310 DEG C is warming up to the heating rate of 1-3 DEG C/min.
Preferably, further including polishing and by silver electrode.
Preferably, described polish and the resulting potsherd of step S7 be specifically polishing to 0.2-0.3mm by silver electrode
Thickness, it is two-sided paint silver paste with silk screen after, then after being heated up and being kept the temperature, with furnace natural cooling, burning infiltration silver electrode obtains finished product.
Preferably, the specific operation process of polishing are as follows:
Obtained potsherd is first polishing to 1mm thickness with 400 mesh waterproof abrasive paper two sides, is then beaten with 600 mesh waterproof abrasive paper two sides
It is milled to 0.6mm thickness, then is polishing to 0.35mm thickness with 1500 mesh waterproof abrasive paper two sides, finally extremely with diamond paste polishing both surfaces
0.2-0.3mm is thick；
Then, polished sample is placed in ultrasonic cleaner (KQ-300E type), using ethyl alcohol as cleaning agent, cleans 10-
15min is subsequently placed in air dry oven and dries.
Preferably, the heating is to be warming up to 650-850 DEG C with the heating rate of 1-5 DEG C/min, heat preservation 0.5-1 is small
When.
Preferably, further including testing procedure.
Preferably, the test, which refers to, tests the crystal structure of sample, Xiang Jie in finished product respectively by test equipment
Structure observes microstructural alternative, the dielectric properties, ferroelectric hysteresis loop of sample, and under Hi-pot test, sample is placed in silicone oil,
Prevent surface-discharge.
The beneficial effects of the present invention are:
The present invention passes through doping (Bi0.5Na0.5)HfO3In NaNbO3Induced synthesis polar nano microcell in ceramics obtains low
Remanent polarization；High saturated polarization is obtained using the hybridism of the 2p track of the 6s and O of Bi；In addition,
(Bi0.5Na0.5)HfO3Incorporation NaNbO can be significantly reduced3The dielectric loss of base ceramics, improves its consistency, reduces its crystal grain
Size, and then its breakdown strength is improved, it is finally obtained while having the ceramic material of high energy storage density and high energy storage efficiency；
The material by ingredient, ball milling, pre-burning, secondary ball milling, granulating and forming, dumping, obtained at burning, polishing and by silver electrode
?；Energy storage density based on ferroelectric hysteresis loop calculating is in 0.99~3.51J/cm3Between, energy storage efficiency is between 60~80.1%；
The material has energy storage density high as a kind of novel energy storage ceramic material, and preparation process is simple, at low cost, pollution-free, easily
In large-scale production the advantages that, have strong practicability；
Meanwhile compared with existing energy storage ceramic material, which has energy storage density high, and preparation process is simple, burns
Wide temperature region is tied, it is at low cost, it is pollution-free, it is easy to the advantages that being mass produced, there is very strong practicability.A new generation be can be used as in skill
Art and economically simultaneous excellent one of important energy storage candidate material.
Detailed description of the invention
Fig. 1 (a) is 0.95NaNbO in the embodiment of the present invention 13-0.05(Bi0.5Na0.5)HfO3The X of ceramics at room temperature is penetrated
Ray diffraction diagram spectrum；Fig. 1 (b) is 0.95NaNbO in the embodiment of the present invention3-0.05(Bi0.5Na0.5)HfO3The scanning electron microscope of ceramics is shone
Piece；Fig. 1 (c) is 0.95NaNbO in the embodiment of the present invention3-0.05(Bi0.5Na0.5)HfO3The ferroelectric hysteresis loop of ceramics.
Fig. 2 (a) is 0.92NaNbO in the embodiment of the present invention 23-0.08(Bi0.5Na0.5)HfO3The X of ceramics at room temperature is penetrated
Ray diffraction diagram spectrum；Fig. 2 (b) is 0.92NaNbO in the embodiment of the present invention3-0.08(Bi0.5Na0.5)HfO3The scanning electron microscope of ceramics is shone
Piece；Fig. 2 (c) is 0.92NaNbO in the embodiment of the present invention3-0.08(Bi0.5Na0.5)HfO3The ferroelectric hysteresis loop of ceramics.
Fig. 3 (a) is 0.89NaNbO in the embodiment of the present invention 33-0.11(Bi0.5Na0.5)HfO3The X of ceramics at room temperature is penetrated
Ray diffraction diagram spectrum；Fig. 3 (b) is 0.89NaNbO in the embodiment of the present invention3-0.11(Bi0.5Na0.5)HfO3The scanning electron microscope of ceramics is shone
Piece；Fig. 3 (c) is 0.89NaNbO in the embodiment of the present invention3-0.11(Bi0.5Na0.5)HfO3The ferroelectric hysteresis loop of ceramics.
Fig. 4 (a) is 0.85NaNbO in the embodiment of the present invention 43-0.15(Bi0.5Na0.5)HfO3The X of ceramics at room temperature is penetrated
Ray diffraction diagram spectrum；Fig. 4 (b) is 0.85NaNbO in the embodiment of the present invention3-0.15(Bi0.5Na0.5)HfO3The scanning electron microscope of ceramics is shone
Piece；Fig. 4 (c) is 0.85NaNbO in the embodiment of the present invention3-0.15(Bi0.5Na0.5)HfO3The ferroelectric hysteresis loop of ceramics.
Specific embodiment
In order to make those skilled in the art be better understood on technical solution of the present invention, with reference to the accompanying drawing and
Embodiment is further described technical solution of the present invention, it should be understood that specific example described herein is only used to
It explains the present invention, is not intended to limit the present invention.
Embodiment 1
S1, weighing is calculated: by analytically pure natrium carbonicum calcinatum, niobium pentaoxide, bismuth oxide and hafnium oxide raw material
Under the conditions of 120 DEG C after drying and processing 15 hours, by chemical formula 0.95NaNbO3-0.05(Bi0.5Na0.5)HfO3In chemistry meter
Amount is poured into ball grinder than weighing above-mentioned each raw material, obtains mixture；
S2, ball milling: by the resulting mixture of step S1 in ethanol with ZrO2Ball is medium planetary ball mill 12 hours, drying
Sieving, obtains dry powder；
S3, pre-burning: the resulting dry powder of step S2 after pre-burning 5 hours, is ground up, sieved in 920 DEG C of air, obtains powder A；
S4, multiple ball milling: by planetary ball mill 12 hours in ethanol the resulting powder A of step S3, after drying, again by powder
Planetary ball mill 12 hours in ethanol successively carry out 3 ball millings and obtain powder material B after final drying；
S5, granulating and forming: polyvinyl alcohol is added by the 5% of powder quality in the resulting powder material B of step S4 and is granulated, will be granulated
Powder afterwards is dry-pressing formed under the pressure of 100MPa, obtains forming biscuit；
S6, dumping: the resulting forming biscuit of step S5 is placed in moderate oven and is warming up to the heating rate of 3 DEG C/min
After 650 DEG C, heat preservation 2 hours, with furnace natural cooling；
S7, at burning: the heating rate of the resulting forming 5 DEG C/min of biscuit of step S6 is warming up to 600 DEG C, then with 3 DEG C/
After the heating rate of min is warming up to 1310 DEG C, heat preservation 2.5 hours, with furnace natural cooling, ceramic of compact piece is obtained；
S8, polishing and by silver electrode: the resulting potsherd of step S7 is polishing to 0.3mm thickness, specifically: the pottery that will be obtained
Tile is first polishing to 1mm thickness with 400 mesh waterproof abrasive paper two sides, is then polishing to 0.6mm thickness with 600 mesh waterproof abrasive paper two sides, then use
1500 mesh waterproof abrasive paper two sides are polishing to 0.35mm thickness, finally with diamond paste polishing both surfaces to 0.2-0.3mm thickness；The present invention
In order to improve the final silk-screen printing quality of product, therefore polishing step is improved, by thickness needed for existing direct polishing
The polishing mode of degree is improved to the mode that substep is polished, and the specific substep using four step rule is polished mode step by step, and direct
The advantage that the mode of polishing compares is: the precision of polishing is high, surfacing, and polishing precision is high, more conducive to silk-screen printing
It is good to carry out；It is beneficial to improve the breakdown electric field of material；
Then, polished sample is placed in ultrasonic cleaner (KQ-300E type), using ethyl alcohol as cleaning agent, cleans 10-
15min is subsequently placed in air dry oven and dries；
It is two-sided paint silver paste with silk screen after, be warming up to 650 DEG C with the heating rate of 5 DEG C/min, after heat preservation 0.5 hour, with
Furnace natural cooling, burning infiltration silver electrode, obtains finished product.
The crystal structure and phase structure of pre-burning powder and ceramics sample are determined using X-ray diffraction analyzer (XRD),
With the microstructural alternative of scanning electron microscope (SEM) observation ceramics sample.It is surveyed with Agilent E4980A LCR test set
Try dielectric properties.Using ferroelectricity analyzer TF-2000, the ferroelectric hysteresis loop of test ceramics and glass ceramics sample.When Hi-pot test,
Sample is placed in silicone oil, surface-discharge is prevented.
Table one is the performance test results of 1 ceramic material of embodiment
Embodiment 2
S1, weighing is calculated: by analytically pure natrium carbonicum calcinatum, niobium pentaoxide, bismuth oxide and hafnium oxide raw material
Under the conditions of 140 DEG C after drying and processing 13 hours, by chemical formula 0.92NaNbO3-0.08(Bi0.5Na0.5)HfO3In chemistry meter
Amount is poured into ball grinder than weighing above-mentioned each raw material, obtains mixture；
S2, ball milling: by the resulting mixture of step S1 in ethanol with ZrO2Ball is medium planetary ball mill 15 hours, drying
Sieving, obtains dry powder；
S3, pre-burning: the resulting dry powder of step S2 after pre-burning 8 hours, is ground up, sieved in 900 DEG C of air, obtains powder A；
S4, multiple ball milling: by planetary ball mill 15 hours in ethanol the resulting powder A of step S3, after drying, again by powder
Planetary ball mill 20 hours in ethanol successively carry out 2 ball millings and obtain powder material B after final drying；
S5, granulating and forming: polyvinyl alcohol is added by the 5% of powder quality in the resulting powder material B of step S4 and is granulated, will be granulated
Powder afterwards is dry-pressing formed under the pressure of 150MPa, obtains forming biscuit
S6, dumping: the resulting forming biscuit of step S5 is placed in moderate oven and is warming up to the heating rate of 2 DEG C/min
After 600 DEG C, heat preservation 3 hours, with furnace natural cooling；
S7, at burning: the heating rate of the resulting forming 4 DEG C/min of biscuit of step S6 is warming up to 600 DEG C, then with 2 DEG C/
After the heating rate of min is warming up to 1280 DEG C, heat preservation 3 hours, with furnace natural cooling, ceramic of compact piece is obtained；
S8, polishing and by silver electrode: the resulting potsherd of step S7 is polishing to 0.25mm thickness, polishing specific steps are the same as real
Apply example 1, it is two-sided paint silver paste with silk screen after, after being warming up to 700 DEG C, heat preservation 0.5 hour with the heating rate of 3 DEG C/min, with furnace
Natural cooling, burning infiltration silver electrode, obtains finished product.
Test method is the same as embodiment 1
Table two is the performance test results of 2 ceramic material of embodiment
Embodiment 3
S1, weighing is calculated: by analytically pure natrium carbonicum calcinatum, niobium pentaoxide, bismuth oxide and hafnium oxide raw material
Under the conditions of 150 DEG C after drying and processing 10 hours, by chemical formula 0.89NaNbO3-0.11(Bi0.5Na0.5)HfO3In chemistry meter
Amount is poured into ball grinder than weighing above-mentioned each raw material, obtains mixture；
S2, ball milling: by the resulting mixture of step S1 in ethanol with ZrO2Ball is medium planetary ball mill 20 hours, drying
Sieving, obtains dry powder；
S3, pre-burning: the resulting dry powder of step S2 after pre-burning 10 hours, is ground up, sieved in 890 DEG C of air, obtains powder A；
S4, multiple ball milling: by planetary ball mill 15 hours in ethanol the resulting powder A of step S3, after drying, again by powder
Planetary ball mill 12 hours in ethanol successively carry out 3 ball millings and obtain powder material B after final drying；
S5, granulating and forming: polyvinyl alcohol is added by the 5% of powder quality in the resulting powder material B of step S4 and is granulated, will be granulated
Powder afterwards is dry-pressing formed under the pressure of 300MPa, obtains forming biscuit；
S6, dumping: the resulting forming biscuit of step S5 is placed in moderate oven and is warming up to the heating rate of 1 DEG C/min
After 500 DEG C, heat preservation 5 hours, with furnace natural cooling；
S7, at burning: the heating rate of the resulting forming 3 DEG C/min of biscuit of step S6 is warming up to 600 DEG C, then with 1 DEG C/
After the heating rate of min is warming up to 1260 DEG C, heat preservation 5 hours, with furnace natural cooling, ceramic of compact piece is obtained；
S8, polishing and by silver electrode: the resulting potsherd of step S7 is polishing to 0.2mm thickness, polishing specific steps are the same as real
Apply example 1, it is two-sided paint silver paste with silk screen after, after being warming up to 650 DEG C, heat preservation 1 hour with the heating rate of 1 DEG C/min, with furnace from
So cooling, burning infiltration silver electrode obtains finished product.
Test method is the same as embodiment 1
Table three is the performance test results of 3 ceramic material of embodiment
Embodiment 4
S1, weighing is calculated: by analytically pure natrium carbonicum calcinatum, niobium pentaoxide, bismuth oxide and hafnium oxide raw material
Under the conditions of 130 DEG C after drying and processing 14 hours, by chemical formula 0.85NaNbO3-0.15(Bi0.5Na0.5)HfO3In chemistry meter
Amount is poured into ball grinder than weighing above-mentioned each raw material, obtains mixture；
S2, ball milling: by the resulting mixture of step S1 in ethanol with ZrO2Ball is medium planetary ball mill 15 hours, drying
Sieving, obtains dry powder；
S3, pre-burning: the resulting dry powder of step S2 after pre-burning 6 hours, is ground up, sieved in 900 DEG C of air, obtains powder A；
S4, multiple ball milling: by planetary ball mill 18 hours in ethanol the resulting powder A of step S3, after drying, again by powder
Planetary ball mill 18 hours in ethanol successively carry out 3 ball millings and obtain powder material B after final drying；
S5, granulating and forming: polyvinyl alcohol is added by the 5% of powder quality in the resulting powder material B of step S4 and is granulated, will be granulated
Powder afterwards is dry-pressing formed under the pressure of 250MPa, obtains forming biscuit；
S6, dumping: the resulting forming biscuit of step S5 is placed in moderate oven and is warming up to the heating rate of 2 DEG C/min
After 620 DEG C, heat preservation 3 hours, with furnace natural cooling；
S7, at burning: the resulting forming biscuit of step S6 is warming up to 600 DEG C with the heating rate of 4 DEG C/min, then with 3 DEG C/
After the heating rate of min is warming up to 1255 DEG C, heat preservation 2 hours, with furnace natural cooling, ceramic of compact piece is obtained；
S8, polishing and by silver electrode: the resulting potsherd of step S47 is polishing to 0.2mm thickness, polishing specific steps are the same as real
Apply example 1, it is two-sided paint silver paste with silk screen after, after being warming up to 800 DEG C, heat preservation 0.5 hour with the heating rate of 3 DEG C/min, with furnace
Natural cooling, burning infiltration silver electrode, obtains finished product.
Test method is the same as embodiment 1
Table four is the performance test results of 4 ceramic material of embodiment
Embodiment 5
S1, weighing is calculated: by analytically pure natrium carbonicum calcinatum, niobium pentaoxide, bismuth oxide and hafnium oxide raw material
Under the conditions of 135 DEG C after drying and processing 12 hours, by chemical formula 0.80NaNbO3-0.20(Bi0.5Na0.5)HfO3In chemistry meter
Amount is poured into ball grinder than weighing above-mentioned each raw material, obtains mixture；
S2, ball milling: by the resulting mixture of step S1 in ethanol with ZrO2Ball is medium planetary ball mill 17 hours, drying
Sieving, obtains dry powder；
S3, pre-burning: the resulting dry powder of step S2 after pre-burning 12 hours, is ground up, sieved in 870 DEG C of air, obtains powder A；
S4, multiple ball milling: by planetary ball mill 16 hours in ethanol the resulting powder A of step S3, after drying, again by powder
Planetary ball mill 16 hours in ethanol successively carry out 2 ball millings and obtain powder material B after final drying；
S5, granulating and forming: polyvinyl alcohol is added by the 5% of powder quality in the resulting powder material B of step S4 and is granulated, will be granulated
Powder afterwards is dry-pressing formed under the pressure of 200MPa, obtains forming biscuit；
S6, dumping: the resulting forming biscuit of step S5 is placed in moderate oven and is warming up to the heating rate of 2.5 DEG C/min
After 580 DEG C, heat preservation 4 hours, with furnace natural cooling；
S7, at burning: the resulting forming biscuit of step S6 is warming up to 600 DEG C with the heating rate of 3.5 DEG C/min, then with 2
DEG C/after the heating rate of min is warming up to 1230 DEG C, heat preservation 4 hours, with furnace natural cooling, obtain ceramic of compact piece；
S8, polishing and by silver electrode: the resulting potsherd of step S57 is polishing to 0.3mm thickness, polishing specific steps are the same as real
Apply example 1, it is two-sided paint silver paste with silk screen after, after being warming up to 800 DEG C, heat preservation 0.5 hour with the heating rate of 3 DEG C/min, with furnace
Natural cooling, burning infiltration silver electrode, obtains finished product.
Test method is the same as embodiment 1
Table five is the performance test results of 5 ceramic material of embodiment
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of ceramic material simultaneously with high energy storage density and efficiency, it is characterised in that: the chemical group of the ceramic material
As (1-x) NaNbO3-x(Bi0.5Na0.5)HfO3, wherein 0.05≤x≤0.2.
2. a kind of preparation method of ceramic material simultaneously with high energy storage density and efficiency as described in claim 1, special
Sign is, comprising the following steps:
S1, it calculates weighing: analytically pure natrium carbonicum calcinatum, niobium pentaoxide, bismuth oxide and hafnium oxide raw material is existed
Under the conditions of 120-150 DEG C after drying and processing 10-15 hours, by chemical general formula (1-x) NaNbO3-x(Bi0.5Na0.5)HfO3, (0.05
≤ x≤0.2) in stoichiometric ratio successively weigh above-mentioned each raw material, and successively pour into ball grinder, obtain mixture；
S2, ball milling: by the resulting mixture of step S1 in ethanol with ZrO2Ball is medium planetary ball mill 12-20 hours, is dried
Sieve, obtains dry powder；
S3, pre-burning: the resulting dry powder of step S2 after pre-burning 5-12 hours, is ground up, sieved in 870-920 DEG C of air, obtains powder
A；
S4, multiple ball milling: by the resulting powder A of step S3 planetary ball mill 12-20 hours in ethanol；
After drying, in ethanol planetary ball mill 12-20 hours again by powder, multiple ball milling is successively carried out, after final drying, obtains powder
Expect B；
S5, granulating and forming: polyvinyl alcohol is added by the 5% of powder quality in the resulting powder material B of step S4 and is granulated, morphogen is obtained
Base；
S6, dumping: the resulting forming biscuit of step S5 being placed in moderate oven after being warming up to 500-650 DEG C, heat preservation 2-5 hours,
With furnace natural cooling；
S7, at burning: the resulting forming biscuit of step S6 is gradually heated to 1230-1310 DEG C using two step temperature-raising methods, keeps the temperature 1-5
After hour, with furnace natural cooling, ceramic of compact piece is obtained.
3. a kind of preparation method of ceramic material simultaneously with high energy storage density and efficiency according to claim 2,
It is characterized in that, the powder after being granulated in the step S5 is dry-pressing formed under the pressure of 100-300MPa.
4. a kind of preparation method of ceramic material simultaneously with high energy storage density and efficiency according to claim 2,
It is characterized in that, the rate that temperature rises in the step S6 is specially 1-3 DEG C/min.
5. a kind of preparation method of ceramic material simultaneously with high energy storage density and efficiency according to claim 2,
It is characterized in that, two step temperature-raising methods in the step S7, which refer to, is warming up to 600 DEG C with the heating rate of 3-5 DEG C/min, then with 1-3
DEG C/heating rate of min is warming up to 1230-1310 DEG C.
6. a kind of preparation method of ceramic material simultaneously with high energy storage density and efficiency according to claim 2,
It is characterized in that, further includes polishing and by silver electrode.
7. a kind of preparation method of ceramic material simultaneously with high energy storage density and efficiency according to claim 6,
It is characterized in that, it is described to polish and the resulting potsherd of step S7 is specifically polishing to by 0.2-0.3mm thickness, two-sided use by silver electrode
After silk screen paints silver paste, then after being heated up and being kept the temperature, with furnace natural cooling, burning infiltration silver electrode obtains finished product.
8. a kind of preparation method of ceramic material simultaneously with high energy storage density and efficiency according to claim 7,
It is characterized in that, the specific operation process of polishing are as follows:
Obtained potsherd is first polishing to 1mm thickness with 400 mesh waterproof abrasive paper two sides, is then polishing to 600 mesh waterproof abrasive paper two sides
0.6mm is thick, then is polishing to 0.35mm thickness with 1500 mesh waterproof abrasive paper two sides, finally with diamond paste polishing both surfaces to 0.2-
0.3mm is thick；
Then, polished sample is placed in ultrasonic cleaner (KQ-300E type), using ethyl alcohol as cleaning agent, cleans 10-
15min is subsequently placed in air dry oven and dries.
9. a kind of preparation method of ceramic material simultaneously with high energy storage density and efficiency according to claim 8,
It is characterized in that, the heating is that 650-850 DEG C is warming up to the heating rate of 1-5 DEG C/min, keeps the temperature 0.5-1 hours.
10. according to a kind of any one of claim 2-9 preparation of the ceramic material simultaneously with high energy storage density and efficiency
Method, which is characterized in that further include testing procedure, the test, which refers to, tests sample in finished product respectively by test equipment
Crystal structure, phase structure observe microstructural alternative, the dielectric properties, ferroelectric hysteresis loop of sample, and under Hi-pot test, by sample
Product are placed in silicone oil, prevent surface-discharge.
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