CN109456055A - A kind of high breakdown high polarization bismuth-sodium titanate ceramic material, preparation method and application - Google Patents
A kind of high breakdown high polarization bismuth-sodium titanate ceramic material, preparation method and application Download PDFInfo
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- 230000010287 polarization Effects 0.000 title claims abstract description 39
- 230000015556 catabolic process Effects 0.000 title claims abstract description 33
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 33
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000919 ceramic Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 13
- 238000005498 polishing Methods 0.000 claims description 13
- 238000000498 ball milling Methods 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 244000137852 Petrea volubilis Species 0.000 claims description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 10
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- 229910052709 silver Inorganic materials 0.000 claims description 10
- 239000004332 silver Substances 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 5
- 239000002003 electrode paste Substances 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- 229910003237 Na0.5Bi0.5TiO3 Inorganic materials 0.000 abstract description 8
- 229910002115 bismuth titanate Inorganic materials 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 230000005684 electric field Effects 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 239000003989 dielectric material Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910010252 TiO3 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C04B35/46—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 titanium oxides or titanates
- C04B35/462—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 titanium oxides or titanates based on titanates
- C04B35/475—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 titanium oxides or titanates based on titanates based on bismuth titanates
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Abstract
本发明提供了一种制备高击穿高极化钛酸铋钠陶瓷的新方法，通过球磨、烘干、微波煅烧、超声粉碎、过筛、冷等静压和微波烧结得到高击穿和高极化的Na0.5Bi0.5TiO3陶瓷样品。本发明提供的陶瓷材料具有高的击穿强度和高的极化强度，且制备工艺简单，易于大规模生产，为制备高击穿和高极化陶瓷材料提供了新方法。
The present invention provides a new method for preparing high-breakdown and high-polarization sodium bismuth titanate ceramics. The high-breakdown and high-pressure Polarized Na 0.5 Bi 0.5 TiO 3 ceramic sample. The ceramic material provided by the invention has high breakdown strength and high polarization strength, and the preparation process is simple, which is easy for large-scale production, and provides a new method for preparing high breakdown and high polarization ceramic materials.
Description
Technical field
The present invention relates to relaxation ferroelectric technical fields, and in particular to a kind of high breakdown high polarization Na0.5Bi0.5TiO3Ceramics
Material, preparation method and application.
Background technique
Ceramic dielectric material is widely used in electricity due to the features such as charge-discharge velocity is fast, power density is high and heat-resisting quantity
In power electronic equipment.Dielectric capacitor occupies 25% volume and weight of power electronic equipment, in order to reduce electronic device
Volume and weight, there is an urgent need to improve the polarization intensity of dielectric material and disruptive field intensity.
Relaxation ferroelectric due to having zero residual polarization (P in the ideal situationr) and high saturated polarization (Ps), it is stored up in energy
It deposits and is received more and more attention in application.But most of relaxation ferroelectrics be all it is leaded, making and using process
In very big damage is caused to environment, it is therefore desirable to develop unleaded relaxor ferroelectric system.
Na0.5Bi0.5TiO3(NBT) be due to its high polarization intensity (P s=43 μC/cm2), it is considered to be one kind has pole
The relaxation ferroelectric of big potentiality.
Summary of the invention
Due to the big atomic weight of Bi element and sintering when volatilization, traditional preparation method hardly result in pure phase and
Uniform bismuth-sodium titanate ceramics, have seriously affected its breakdown strength and polarization intensity.The purpose of the present invention is to provide a kind of high
The preparation method of breakdown and high polarization medium ceramic material, to overcome the problems of the above-mentioned prior art.Using of the invention
The ceramics that method obtains have high breakdown and high polarization, and preparation process is simple, and the cost of material is low, are easy to be mass produced,
It is environmental-friendly, new method is provided for the high breakdown of preparation and high polarization ceramic material.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of high energy-storing dielectric ceramic material, stoichiometric equation are as follows: Na0.5Bi0.5TiO3。
And the preparation method of above-mentioned medium ceramic material, comprising the following steps:
A kind of preparation method of high breakdown high polarization bismuth-sodium titanate ceramic material, which comprises the following steps:
Step 1: Na is weighed first, in accordance with molar ratio 1:1:42CO3、Bi2O3And TiO2It is mixed to form mixture A.
Step 2: and then agate is put into after taking mixture A, zirconium ballstone and dehydrated alcohol to mix according to mass ratio for 1:5:1
Ball milling 6-8 h is carried out in ball grinder, obtains mixture B.
Step 3:, by mixture C drying, sieving, microwave calcination obtain powder D.
Step 4: by powder D, according to the requirement of step 2 and step 3, ball milling, drying, sieving and microwave calcination are obtained again
To powder E.
Step 4: powder E is homogenized in supersonic cleaning machine, and powder F is obtained after drying.
Step 5: powder F is sieved, and isostatic cool pressing obtains green body G.
Step 6: green body G is put into sintering in microwave agglomerating furnace and obtains bismuth-sodium titanate ceramics.
Further, the drying temperature of step 3 and step 4 is 80 DEG C, is sieved selection criteria sub-sieve (40 mesh), microwave
Calcining carries out in microwave agglomerating furnace, detailed process are as follows: 30 min keep the temperature 5 at 700 DEG C from room temperature to 700 DEG C
Min, subsequent furnace cooling.
Further, the ultrasound homogenization in step 4, in supersonic cleaning machine, by powder E and dehydrated alcohol according to body
Product is placed in beaker than 1:2, a length of 5 h when ultrasonic.
Further, the specific preparation feature of the green body G in step 5 is as follows, and be sieved selection criteria sub-sieve (120-200
Mesh), the design parameter of isostatic cool pressing is 200-250 MPa, 3-5 min.
Further, be sintered in step 6, in microwave agglomerating furnace, detailed process is as follows: 30 min are warming up to 900 DEG C,
1040 DEG C are warming up to using 15 min, 5 min are kept the temperature at 1040 DEG C, then furnace cooling.
Further, a kind of application of high breakdown high polarization ceramic material as Lead-free ferroelectric ceramics material, feature exist
In: polishing, cleaning sintering ceramics coat silver electrode paste in sintering ceramic surface, the ceramic material for coating silver electrode are carried out
Sintering obtains the bismuth-sodium titanate ceramics of high breakdown high polarization.
Further, a kind of application of high breakdown high polarization ceramic material as Lead-free ferroelectric ceramics material, feature exist
It is first then to be beaten to 0.3 mm with 2000 mesh sand paper front and back sides with 240 mesh sand paper polishing thickness of sample in the requirement of polishing sample
It is milled to a thickness of 0.2mm.
Compared with prior art, the invention has the following beneficial technical effects:
The Na of the method for the present invention preparation0.5Bi0.5TiO3Ceramic material not only has high breakdown strength and polarization intensity, and makes
Standby simple process, the cost of material is low, environmentally protective, becomes substitution lead base ceramic material and is used as high-end industrial application material in technology
Economically simultaneous excellent important candidate material.
Detailed description of the invention
Fig. 1 is (1-x)Na0.5Bi0.5TiO3The XRD spectrum and SEM of ceramic material are schemed；
Fig. 2 is (1-x)Na0.5Bi0.5TiO3The ceramic material not P-E loops under same electric field；
Fig. 3 is (1-x)Na0.5Bi0.5TiO3P-E loops under ceramic material different frequency.
Specific embodiment
Embodiments of the present invention are described in further detail below:
A kind of preparation method of high breakdown high polarization bismuth-sodium titanate ceramic material, comprising the following steps:
Step 1: Na is weighed first, in accordance with molar ratio 1:1:42CO3、Bi2O3And TiO2It is mixed to form mixture A.
Step 2: and then agate is put into after taking mixture A, zirconium ballstone and dehydrated alcohol to mix according to mass ratio for 1:5:1
Ball milling 6-8 h is carried out in ball grinder, obtains mixture B.
Step 3:, by mixture C 80 DEG C drying, selection criteria sub-sieve (40 mesh) sieving, microwave calcination microwave burn
It is carried out in freezing of a furnace, detailed process are as follows: 30 min keep the temperature 5 min from room temperature to 700 DEG C at 700 DEG C, then cold with furnace
But.Obtain powder D.
Step 4: by powder D, according to the requirement of step 2 and step 3, ball milling, drying, sieving and microwave calcination are obtained again
To powder E.
Step 4: by powder E in supersonic cleaning machine, powder E and dehydrated alcohol are placed on burning according to volume ratio 1:2
In cup, a length of 5 h when ultrasonic., powder F is obtained after drying.
Step 5: powder F is sieved, and is sieved selection criteria sub-sieve (120-200 mesh), and it is quiet that further progress is cold etc.
Pressure, the design parameter of isostatic cool pressing are 200-250 MPa, 3-5 min.Obtain green body G.
Step 6: sintered body G, in microwave agglomerating furnace, detailed process is as follows: 30 min are warming up to 900 DEG C, using
15 min are warming up to 1040 DEG C, 5 min are kept the temperature at 1040 DEG C, then furnace cooling.
Step 7: it is first then polishing to 0.3 mm with 2000 mesh sand paper front and back sides with 240 mesh sand paper polishing thickness of sample
With a thickness of 0.2mm.Cleaning sintering ceramics coat silver electrode paste in sintering ceramic surface, will coat the ceramic material of silver electrode
It is sintered, obtains the bismuth-sodium titanate ceramics of high breakdown high polarization.
Below with reference to embodiment, the invention will be described in further detail, it should be understood that following specific embodiments
It is only for of the invention further elucidated above, rather than to further limitation of the invention:
Embodiment 1
A kind of preparation method of high breakdown high polarization bismuth-sodium titanate ceramic material, comprising the following steps:
Step 1: Na is weighed first, in accordance with molar ratio 1:1:42CO3、Bi2O3And TiO2It is mixed to form mixture A.
Step 2: and then agate is put into after taking mixture A, zirconium ballstone and dehydrated alcohol to mix according to mass ratio for 1:5:1
6 h of ball milling is carried out in ball grinder, obtains mixture B.
Step 3:, by mixture C 80 DEG C drying, selection criteria sub-sieve (40 mesh) sieving, microwave calcination microwave burn
It is carried out in freezing of a furnace, detailed process are as follows: 30 min keep the temperature 5 min from room temperature to 700 DEG C at 700 DEG C, then cold with furnace
But.Obtain powder D.
Step 4: by powder D, according to the requirement of step 2 and step 3, ball milling, drying, sieving and microwave calcination are obtained again
To powder E.
Step 4: by powder E in supersonic cleaning machine, powder E and dehydrated alcohol are placed on burning according to volume ratio 1:2
In cup, a length of 5 h when ultrasonic., powder F is obtained after drying.
Step 5: powder F is sieved, and is sieved selection criteria sub-sieve (120 mesh), further progress isostatic cool pressing,
The design parameter of isostatic cool pressing is 200MPa, 3 min.Obtain green body G.
Step 6: sintered body G, in microwave agglomerating furnace, detailed process is as follows: 30 min are warming up to 900 DEG C, using
15 min are warming up to 1040 DEG C, 5 min are kept the temperature at 1040 DEG C, then furnace cooling.
Step 7: it is first then polishing to 0.3 mm with 2000 mesh sand paper front and back sides with 240 mesh sand paper polishing thickness of sample
With a thickness of 0.2mm.Cleaning sintering ceramics coat silver electrode paste in sintering ceramic surface, will coat the ceramic material of silver electrode
It is sintered, obtains the bismuth-sodium titanate ceramics of high breakdown high polarization.
Embodiment 2
A kind of preparation method of high breakdown high polarization bismuth-sodium titanate ceramic material, comprising the following steps:
Step 1: Na is weighed first, in accordance with molar ratio 1:1:42CO3、Bi2O3And TiO2It is mixed to form mixture A.
Step 2: and then agate is put into after taking mixture A, zirconium ballstone and dehydrated alcohol to mix according to mass ratio for 1:5:1
8 h of ball milling is carried out in ball grinder, obtains mixture B.
Step 3:, by mixture C 80 DEG C drying, selection criteria sub-sieve (40 mesh) sieving, microwave calcination microwave burn
It is carried out in freezing of a furnace, detailed process are as follows: 30 min keep the temperature 5 min from room temperature to 700 DEG C at 700 DEG C, then cold with furnace
But.Obtain powder D.
Step 4: by powder D, according to the requirement of step 2 and step 3, ball milling, drying, sieving and microwave calcination are obtained again
To powder E.
Step 4: by powder E in supersonic cleaning machine, powder E and dehydrated alcohol are placed on burning according to volume ratio 1:2
In cup, a length of 5 h when ultrasonic., powder F is obtained after drying.
Step 5: powder F is sieved, and is sieved selection criteria sub-sieve (200 mesh), further progress isostatic cool pressing,
The design parameter of isostatic cool pressing is 250 MPa, 5 min.Obtain green body G.
Step 6: sintered body G, in microwave agglomerating furnace, detailed process is as follows: 30 min are warming up to 900 DEG C, using
15 min are warming up to 1040 DEG C, 5 min are kept the temperature at 1040 DEG C, then furnace cooling.
Step 7: it is first then polishing to 0.3 mm with 2000 mesh sand paper front and back sides with 240 mesh sand paper polishing thickness of sample
With a thickness of 0.2mm.Cleaning sintering ceramics coat silver electrode paste in sintering ceramic surface, will coat the ceramic material of silver electrode
It is sintered, obtains the bismuth-sodium titanate ceramics of high breakdown high polarization.
Embodiment 3
XRD and SEM test is carried out to sample prepared by embodiment 1, obtains Fig. 1 as a result, Fig. 1 is Na0.5Bi0.5TiO3Ceramics
XRD spectrum and SEM figure, illustration are the optical photograph of sample.It will be seen from figure 1 that the perovskite that pure phase is presented in all samples is brilliant
Body structure illustrates that we have prepared purer ceramics sample without apparent second phase.SEM shows that ceramics sample has
Fine and close microstructure, from illustration it can be seen that ceramics sample has certain translucency.
To its not P-E loops under same electric field of 1 sample test of embodiment, Fig. 2 result is obtained.Figure it is seen that
With being continuously increased for electric field, P-E loops is constantly stretched, and breakdown strength and polarization intensity are continuously increased, and passes through the party
The breakdown strength and polarization intensity of the bismuth-sodium titanate ceramics of method preparation are up to 150 kV/cm and 65 μ C/cm respectively3, and document
The breakdown and polarization of middle report are 120 kV/cm and 43 μ C/cm3。
To the P-E loops under its different frequency of 2 sample test of embodiment, Fig. 3 result is obtained.As can be seen from Figure 3 with
The variation of frequency, polarization intensity there is certain stability, and frequency is higher, and polarization intensity has slight reduction.
Claims (9)
1. a kind of preparation method of high breakdown high polarization bismuth-sodium titanate ceramic material, which comprises the following steps:
Na2CO3、Bi2O3、TiO21:1:4 is mixed in molar ratio；Ball milling 6-8 h, 700 DEG C of 5 min of microwave calcination；Repeat aforementioned ball
Mill, microwave calcination step；Powder is homogenized in supersonic cleaning machine, is dried；Powder is sieved, isostatic cool pressing obtains
Green body；Green body is heated to 900 DEG C, 1040 DEG C is warming up to from 900 DEG C by 15 min, 5 min microwaves is kept the temperature at 1040 DEG C
Sintering obtains bismuth-sodium titanate ceramics.
2. a kind of preparation method of high breakdown high polarization bismuth-sodium titanate ceramic material according to claim 1, feature exist
In specific steps include:
Step 1: Na is weighed first, in accordance with molar ratio 1:1:42CO3、Bi2O3And TiO2It is mixed to form mixture A；
Step 2: and then agate ball milling is put into after taking mixture A, zirconium ballstone and dehydrated alcohol to mix according to mass ratio for 1:5:1
Ball milling 6-8 h is carried out in tank, obtains mixture B；
Step 3: mixture C drying, sieving, microwave calcination are obtained into powder D；
Step 4: by powder D, according to the requirement of step 2 and step 3, ball milling, drying, sieving and microwave calcination obtain powder again
Body E；
Step 5: powder E is homogenized in supersonic cleaning machine, and powder F is obtained after drying；
Step 6: powder F is sieved, and isostatic cool pressing obtains green body G；
Step 7: green body G is put into sintering in microwave agglomerating furnace and obtains bismuth-sodium titanate ceramics.
3. a kind of preparation method of high breakdown high polarization bismuth-sodium titanate ceramic material according to claim 2, feature exist
In the specific preparation process of the powder E of step 4 is as follows: drying temperature is 80 DEG C；Be sieved 40 mesh of selection criteria sub-sieve；Microwave
Calcining carries out in microwave agglomerating furnace；Detailed process are as follows: 30 min keep the temperature 5 min from room temperature to 700 DEG C at 700 DEG C,
Subsequent furnace cooling.
4. a kind of preparation method of high breakdown high polarization bismuth-sodium titanate ceramic material according to claim 2, feature exist
In the ultrasound in step 5 homogenizes, and in supersonic cleaning machine, powder E and dehydrated alcohol are placed on burning according to volume ratio 1:2
In cup, a length of 5 h when ultrasonic.
5. a kind of preparation method of high breakdown high polarization bismuth-sodium titanate ceramic material according to claim 2, feature exist
In the specific preparation process of the green body G in step 6 is as follows: the quasi- sub-sieve sieving of selection 120-200 target, the tool of isostatic cool pressing
Body parameter is 200-250 MPa, 3-5 min.
6. a kind of preparation method of high breakdown high polarization bismuth-sodium titanate ceramic material according to claim 2, feature exist
In be sintered in step 7, in microwave agglomerating furnace, detailed process is as follows: 30 min are warming up to 900 DEG C, using 15 min liters
Temperature keeps the temperature 5 min, then furnace cooling to 1040 DEG C at 1040 DEG C.
7. a kind of high breakdown high polarization bismuth-sodium titanate ceramic material of any one of claim 1 ~ 6 the method preparation.
8. a kind of high breakdown high polarization bismuth-sodium titanate ceramic material answering as Lead-free ferroelectric ceramics material described in claim 7
With, which is characterized in that polishing, cleaning sintering ceramics coat silver electrode paste in sintering ceramic surface, will coat the pottery of silver electrode
Ceramic material is sintered, and obtains the bismuth-sodium titanate ceramics of high breakdown high polarization.
9. a kind of high breakdown high polarization bismuth-sodium titanate ceramic material is as Lead-free ferroelectric ceramics material according to claim 8
Using, which is characterized in that the requirement for sample of polishing is, first with 240 mesh sand paper polishing thickness of sample to 0.3 mm, then with 2000
Mesh sand paper front and back sides are polishing to a thickness of 0.2mm.
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