CN105523760B - A kind of preparation method of the sodium niobate ceramic material of the low-dielectric loss of stable anti-ferroelectricity - Google Patents
A kind of preparation method of the sodium niobate ceramic material of the low-dielectric loss of stable anti-ferroelectricity Download PDFInfo
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Abstract
A kind of preparation method of the sodium niobate ceramic material of the low-dielectric loss of stable anti-ferroelectricity, belongs to dielectric ceramic material field.The stabilization that antiferroelectric phase in pure sodium niobate ceramics is realized by this method, do not occur under the high electric field of 100kV/cm yet electric field induction ferroelectric phase, while material have low-dielectric loss (<2%).Preparation method：Amount is than being Na by mol:Nb=1:1 weighs Na2CO3And Nb2O5, two kinds of raw materials are put into ball milling in ball grinder, absolute ethyl alcohol does abrasive media；The powder that subsequent batch mixing obtains dry grinds to obtain sodium niobate nanometer powder by high-energy ball milling method, obtained nano-powder is not added under the premise of any binder after direct weighting molding, 1350~1375 DEG C sinter ceramic body into.The determination for stablizing antiferroelectric phase is obtained by electric performance test.The method of the present invention is simple, and low energy consumption；Prepared sodium niobate ceramic material has relatively stable anti-ferroelectricity and low-dielectric loss.
Description
Technical field
The invention belongs to sodium niobate technical field of ceramic material, and in particular to a kind of low-dielectric loss of stable anti-ferroelectricity
Sodium niobate ceramic material preparation method.
Background technology
Sodium niobate (NaNbO3) it is both key component in a variety of leadless electronic ceramic systems, pure phase is again because of antiferroelectric knot
Structure and it is with important application prospects in fields such as energy-storage capacitor, high voltage power supply capacitors.Although theoretically pure sodium niobate exists
It is antiferroelectric phase under room temperature, but sodium niobate ceramics prepared by conventional ceramic technique is used to be lacked due to the volatilization of alkali metal
It loses, Lacking oxygen and alkali metal cation vacancy easily occurs, these vacancy form disfigurement model pair, are easily induced under weak electric field
Sodium niobate changes (Ge et al., J.Am.Ceram.Soc., 94,4329-4334 (2011)) from antiferroelectric to ferroelectric.Cause
And the sodium niobate base ceramic systems in document report are difficult to observe antiferroelectric behavior.In order to obtain stable antiferroelectric phase, outside
It is a kind of important method to add the introducing of the second constituent element stabilizer.Shimizu and Guo et al. pass through CaZrO3Or SrZrO3Second group
Member introducing come reduce the system tolerance factor and improve average electronegativity, and then stablize antiferroelectric phase (Shimizu et al.,
Dalton Trans.44,10763(2015)and Guo et al.,J.Appl.Phys.117,214103(2015)).But
What this method of modifying obtained is the antiferroelectric system of binary complex phase.In order to obtain stable antiferroelectric pure sodium niobate unit phase,
Calcining and sintering process inhibit the volatilization of alkali metallic sodium under Shimizu et al. application hypoxic atmospheres, but its result of study still fails
Obtain stable antiferroelectric phase (Shimizu et al., J.Am.Ceram.Soc., 97 [6] 1791-1796 (2014)).In addition,
It should be noted that obtain practical application, sodium niobate ceramics also need to have lower dielectric loss (<2%) to inhibit member
The calorific value of device at work.
High-energy-milling and powder embedded sintering technique are combined by the present invention, and sodium niobate nano is prepared by high-energy ball milling method
Powder realizes that ball milling, at phase, to obtain the high-activity nano powder of narrow particle size distribution, and then passes through buried powder without one step of calcining
Sintering process inhibits the volatilization of sodium under high temperature, prepares high-compactness, low defect, the sodium niobate ceramic material of low-dielectric loss.Electricity
Performance test prove obtain stablizes antiferroelectric polarization behavior, until high-voltage breakdown electric field do not occur it is antiferroelectric --- ferroelectricity behavior
Transformation.
Invention content
The object of the present invention is to provide a kind of preparation method of the sodium niobate ceramics of the low-dielectric loss of stable anti-ferroelectricity,
Using this method prepare material have high-compactness, low defect, low-dielectric loss (<2%), while the anti-iron relatively stablized is showed
Electric phase.
To achieve the goals above, the present invention prepares sodium niobate nanometer powder using high-energy ball milling method.At ambient temperature
One step of short time need not be heated at high temperature at phase compared with traditional calcine technology in closed container, and narrow granularity may be implemented
The synthesis of distribution and high-activity nano powder, while inhibiting the volatilization of the alkali metallic sodium in precursor powder preparation process.Then, right
It is to doing a protective atmosphere in sintering process, inhibiting that the sintering process of ceramics sample, which uses powder embedded sintering technique, powder embedded sintering,
The volatilization of alkali metallic sodium prevents the imbalance of material metering ratio, realizes high-compactness, low-dielectric loss, stoichiometric ratio sodium niobate
The reliable preparation of ceramics, to finally obtain stable antiferroelectric phase.In the niobic acid ceramic material of usual non-stoichiometric by
In the volatilization of sodium will produce Lacking oxygen the defects of, these defects form dipole to hindering the densification of ceramic body, and induce anti-
Ferroelectricity --- ferroelectricity changes.
A kind of preparation method of the sodium niobate ceramic material of the low-dielectric loss of stable anti-ferroelectricity, which is characterized in that packet
Include following steps：
(1) chemical formula NaNbO is pressed3A mole metering compare Na:Nb=1:1 weighs Na2CO3And Nb2O5Powder is placed in ball milling
In tank, ball milling obtains uniformly mixed powder after 12 hours.Due to Na2CO3It is hygroscopic, in order to ensure batching metering ratio,
Na2CO3It is dried at 200 DEG C using preceding, and it is the abrasive media of batch mixing to select absolute ethyl alcohol.Na2CO3And Nb2O5It is micron
Grade powder.
(2) powder that step (1) obtains is weighed into ball milling in merging high-energy ball milling tank, ball milling condition by fixed ratio of grinding media to material
For：Ratio of grinding media to material is 15:1~30:1,600~1000/min of rotational speed of ball-mill, 30~120min of Ball-milling Time obtain nanoscale
Ceramic powder；Its reaction process is as follows：
Na2CO3+Nb2O5→2NaNbO3+CO2↑
There is the continuous particle size for hitting broken powder due to abrading-ball to be down to nanoscale in the process, collides in addition
Mechanical energy be constantly passed in powder, to make mixed powder that diffusion reaction occur on nanoscale, be finally completed above-mentioned
Reaction.
Ball milling condition is preferably：Ratio of grinding media to material is 20:The powder obtained when 1, rotational speed of ball-mill 800/min, Ball-milling Time 90min
Sample is best at phase effect and size dispersity, and size distribution is 12~20nm sodium niobate nanometer powders；Therefore preferred ball
This powder is ground as the ceramic post sintering precursor powder in the present invention.
(3) step (2) is obtained into ceramic powder and is directly compressed into green body, be not added with any binder.
(4) green body obtained to step (3) is sintered, and sintering condition is：The rate of 7 DEG C/min rises to 650 from room temperature
DEG C, then the rate of 3.4 DEG C/min rises to 950 DEG C, then 4 DEG C/min rate rise to after 1350~1375 DEG C of heat preservations 2 hours with
Stove is cooled to room temperature；Green body is embedded in step (2) obtained powder in sintering process simultaneously, is sintered.
The above-mentioned material of the present invention has relatively stable antiferroelectric phase.Wherein best sample is the pottery that 1365 DEG C of sintering obtain
Porcelain sample, consistency is up to 98%, room temperature dielectric constant εr=397, tan δ=1.3% is lost in room temperature dielectric, meets high-quality
Amount ceramics require.
Compared with other inventions, the present invention has following remarkable advantage：
(1) this method is by the way that niobium pentaoxide that is cheap, being easily obtained and sodium carbonate to be simply mixed, in room temperature item
So that ballmilling energy is transferred in mixed powder under part and obtains target powder in the short time.This largely reduce material at
This, simplifies the complexity of preparation process.
(2) in the present invention, selection high-energy ball milling method prepares nano-powder.Traditional Method high-temperature calcination is prepared in powder process
The powder granule size that can not be avoided the volatilization of a part of alkali metallic sodium and obtain is larger, poor activity；And high-energy ball milling method is
The synthesis for completing target phase powder in a closed container at ambient temperature avoids alkali metallic sodium caused by heating
Volatilization.In addition, nanometer grade powder has higher sintering activity and defect concentration, be conducive to the sintering densification in later stage.Rear
We further take powder embedded sintering method in the sintering process of phase, and buried powder mainly plays protection in sintering process to green body
The volatilization of alkali metallic sodium in green body is alleviated in the effect of atmosphere, high-densit to realize, low-dielectric loss (<2%) sodium niobate pottery
The preparation of porcelain.
(3) the dielectric properties test data of the sodium niobate ceramics sample of low-dielectric loss obtained by this method is in addition to obtaining public affairs
The T recognizedCT=100 DEG C or so one new dielectric peak, existing text of the peak in sodium niobate is also obtained in=370 DEG C of Curie peak
It was never reported in offering.The appearance at this exception dielectric peak illustrates room temperature with the presence of stable antiferroelectric phase, and electrical testing is shown
The double ferroelectric hysteresis loops of the beam waist type burner of antiferroelectric feature, and test antiferroelectric there are no occurring when electric field is added to 100kv/cm
To the phase transformation of ferroelectricity, indicate that sodium niobate anti-ferroelectricity can be stablized.
Description of the drawings
Fig. 1：Ratio of grinding media to material is 20:The X-ray of the powder sample obtained when 1, rotational speed of ball-mill 800/min, Ball-milling Time 90min
Diffraction (XRD) collection of illustrative plates.
Fig. 2：Ratio of grinding media to material is 20:The powder sample attached drawing obtained when 1, rotational speed of ball-mill 800/min, Ball-milling Time 90min：
(a) low power number transmission electron microscope picture；(b) EDS power spectrums；(c) high magnification numbe transmission electron microscope picture, (d) selective electron diffraction figure.
Fig. 3：The ceramics sample attached drawing that embodiment 2 obtains：
(a) scanning electron microscope (SEM) photograph, (b) grain size distribution figure
Fig. 4：The X ray diffracting spectrum (XRD) for the ceramics sample that embodiment 2 obtains.
Fig. 5：Jie's temperature curve and damage curve of the ceramics sample that embodiment 2 obtains at different frequencies.
Fig. 6：The P-E loop lines of the ceramics sample that embodiment 2 obtains at room temperature.
Specific implementation mode
Below by embodiment the substantive distinguishing features and remarkable advantage that the present invention is furture elucidated, but the present invention is not limited to
Following embodiment.
Synthesize NaNbO3Precursor powder, the precursor powder use Na2CO3And Nb2O5Low price raw material is made, and reaction process is such as
Under：Na2CO3+Nb2O5→2NaNbO3+CO2↑(1)
First by Na2CO3It is dried at 200 DEG C 12 hours, then amount ratio is Na by mol:Nb=1:1 weighs
Na2CO3And Nb2O5In two kinds of raw material merging ball grinders, batch mixing 12 hours in planetary ball mill；The powder that batch mixing obtains is by solid
Determine ratio of grinding media to material and weigh ball milling in merging high-energy ball milling tank, ball milling condition is：Ratio of grinding media to material is 15:1~20:1, rotational speed of ball-mill 600~
1000/min, 30~120min of Ball-milling Time；There is the continuous particle size for hitting broken powder due to abrading-ball in the process
It is down to nanoscale, the mechanical energy generated in another plus collision is constantly passed in powder, to make mixed powder in nanoscale
Upper generation solid diffusion reaction, is finally completed reaction in above-mentioned reaction equation (1).Na2CO3It is easy to absorb water, is unfavorable for the short time into phase
Purpose, therefore it is the abrasive media of batch mixing to select absolute ethyl alcohol.
Na2CO3And Nb2O5It is micron-sized powder.
Embodiment 1：
It is by ball milling condition：Ratio of grinding media to material is 15:High-energy ball milling system when 1, rotational speed of ball-mill 1000/min, Ball-milling Time 90min
Standby obtained NaNbO3Under the premise of powder is not added with any binder, directly in the forming under the pressure of 800MPa, a diameter of 11.5
Millimeter, thickness are 1.5 millimeters or so；Then the rate of 7 DEG C/min rises to 650 DEG C from room temperature, then the rate liter of 3.4 DEG C/min
To 950 DEG C, then the rate of 4 DEG C/min rises to 1350 DEG C of powder embedded sinterings, and heat preservation 2 hours is to get to target ceramic material.
Embodiment 2：
It is by ball milling condition：Ratio of grinding media to material is 20:When 1, rotational speed of ball-mill 800/min, Ball-milling Time 90min prepared by high-energy ball milling
Obtained NaNbO3Under the premise of powder is not added with any binder, directly in the forming under the pressure of 800MPa, a diameter of 11.5 milli
Rice, thickness are 1.5 millimeters or so；Then the rate of 7 DEG C/min rises to 650 DEG C from room temperature, and then the rate of 3.4 DEG C/min rises to
950 DEG C, then the rate of 4 DEG C/min rises to 1365 DEG C of powder embedded sinterings, heat preservation 2 hours is to get to target ceramic material.From Figures 5 and 6
It can be seen that T=100 DEG C or so one new dielectric peak, which never reported in the existing document of sodium niobate.It is this different
The appearance at the peaks Chang Jie electricity illustrates room temperature with the presence of stable antiferroelectric phase, and electrical testing shows that the beam waist type burner of antiferroelectric feature is double
Ferroelectric hysteresis loop, and test when electric field is added to 100kV/cm there are no there is the antiferroelectric phase transformation to ferroelectricity, indicate niobium
Sour sodium anti-ferroelectricity can be stablized.
Embodiment 3：
It is by ball milling condition：Ratio of grinding media to material is 30:High-energy ball milling system when 1, rotational speed of ball-mill 600/min, Ball-milling Time 120min
Standby obtained NaNbO3Under the premise of powder is not added with any binder, directly in the forming under the pressure of 800MPa, a diameter of 11.5
Millimeter, thickness are 1.5 millimeters or so；Then the rate of 7 DEG C/min rises to 650 DEG C from room temperature, and the rate of 3.4 DEG C/min rises to
950 DEG C, then the rate of 4 DEG C/min rises to 1375 DEG C of powder embedded sinterings, heat preservation 2 hours is to get to target ceramic material.
Comparative example 1：
It is by ball milling condition：Ratio of grinding media to material is 20:When 1, rotational speed of ball-mill 800/min, Ball-milling Time 90min prepared by high-energy ball milling
Obtained NaNbO3Under the premise of powder is not added with any binder, directly in the forming under the pressure of 800MPa, a diameter of 11.5 milli
Rice, thickness are 1.5 millimeters or so；Then the rate of 7 DEG C/min rises to 650 DEG C from room temperature, and then the rate of 3.4 DEG C/min rises to
950 DEG C, then the rate of 4 DEG C/min rises to 1330 DEG C of sintering, heat preservation 2 hours is to get to target ceramic material.
Comparative example 2：
It is by ball milling condition：Ratio of grinding media to material is 20:When 1, rotational speed of ball-mill 800/min, Ball-milling Time 90min prepared by high-energy ball milling
Obtained NaNbO3Under the premise of powder is not added with any binder, directly in the forming under the pressure of 800MPa, a diameter of 11.5 milli
Rice, thickness are 1.5 millimeters or so；Then the rate of 7 DEG C/min rises to 650 DEG C from room temperature, and then the rate of 3.4 DEG C/min rises to
950 DEG C, then the rate of 4 DEG C/min rises to 1380 DEG C of powder embedded sinterings, heat preservation 2 hours is to get to target ceramic material.
Comparative example 3：
It is by ball milling condition：Ratio of grinding media to material is 30:High-energy ball milling system when 1, rotational speed of ball-mill 400/min, Ball-milling Time 120min
Standby obtained NaNbO3Under the premise of powder is not added with any binder, directly in the forming under the pressure of 800MPa, a diameter of 11.5
Millimeter, thickness are 1.5 millimeters or so；Then the rate of 7 DEG C/min rises to 650 DEG C from room temperature, then the rate liter of 3.4 DEG C/min
To 950 DEG C, then the rate of 4 DEG C/min rises to 1365 DEG C of sintering, and heat preservation 2 hours is to get to target ceramic material.
The correlation performance parameters contrast table of 1 above-described embodiment of table and comparative example ceramics sample
| Relative density | Dielectric constant | Dielectric loss | Anti-ferroelectricity | |
| Comparative example 1 | 83% | 200 | 46% | Have |
| Comparative example 2 | 93% | 308 | 5.7% | Have |
| Comparative example 3 | 89% | 171 | 39% | Nothing |
| Embodiment 1 | 95% | 285 | 1.64% | Have |
| Embodiment 2 | 98% | 397 | 1.3% | Have |
| Embodiment 3 | 96% | 373 | 1.89% | Have |
Claims (4)
1. a kind of preparation method of the sodium niobate ceramic material of the low-dielectric loss of stable anti-ferroelectricity, which is characterized in that including
Following steps：
(1) chemical formula NaNbO is pressed3A mole metering compare Na:Nb=1:1 weighs Na2CO3And Nb2O5Powder is placed in ball grinder
In, ball milling obtains uniformly mixed powder after 12 hours；Na2CO3It is dried at 200 DEG C using preceding, and selects the absolute ethyl alcohol to be
The abrasive media of batch mixing；Na2CO3And Nb2O5It is micron-sized powder；
(2) powder that step (1) obtains is weighed into ball milling in merging high-energy ball milling tank by fixed ratio of grinding media to material, ball milling condition is：Ball
Material is than being 15:1~30:1,600~1000r/min of rotational speed of ball-mill, 30~120min of Ball-milling Time obtain the ceramics of nanoscale
Powder；Its reaction process is as follows：
Na2CO3+Nb2O5→2NaNbO3+CO2↑；
(3) step (2) is obtained into ceramic powder and is directly compressed into green body, be not added with any binder；
(4) green body obtained to step (3) is sintered, and sintering condition is：The rate of 7 DEG C/min rises to 650 DEG C from room temperature, so
The rate of 3.4 DEG C/min rises to 950 DEG C afterwards, then the rate of 4 DEG C/min rises to furnace cooling after 1350~1375 DEG C of heat preservations 2 hours
To room temperature；Green body is embedded in step (2) obtained powder in sintering process simultaneously, is sintered.
2. a kind of preparation side of the sodium niobate ceramic material of the low-dielectric loss of stable anti-ferroelectricity described in accordance with the claim 1
Method, which is characterized in that step (2) ball milling condition is：Ratio of grinding media to material is 20:When 1, rotational speed of ball-mill 800r/min, Ball-milling Time 90min
Powder is obtained, size distribution is 12~20nm sodium niobate nanometer powders.
3. a kind of preparation side of the sodium niobate ceramic material of the low-dielectric loss of stable anti-ferroelectricity described in accordance with the claim 1
Method, which is characterized in that step (4) rises to 1365 DEG C and keeps the temperature 2 hours.
4. the sodium niobate of the low-dielectric loss for the stabilization anti-ferroelectricity being prepared according to the either method described in claim 1-3
Ceramic material.
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| CN107056291B (en) * | 2017-04-14 | 2020-09-25 | 北京工业大学 | Sub-micron crystal scale piezoelectric energy collecting material and preparation method thereof |
| CN109809815B (en) * | 2019-03-18 | 2021-10-01 | 中国科学院上海硅酸盐研究所 | Lead-free sodium niobate-based antiferroelectric ceramic with high saturation polarization and low residual polarization and preparation method thereof |
| CN110981479B (en) * | 2020-01-10 | 2022-03-01 | 陕西科技大学 | High-breakdown ferroelectric ceramic and preparation method thereof |
| CN115159983B (en) * | 2022-07-01 | 2023-03-10 | 中国科学院上海硅酸盐研究所 | Sodium niobate-based relaxor antiferroelectric ceramic material and preparation method thereof |
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|---|---|---|---|---|
| CN101514103A (en) * | 2009-04-03 | 2009-08-26 | 西北工业大学 | Method for preparing potassium-sodium niobate-sodium bismuth titanate nano ceramics |
| CN101774642A (en) * | 2010-01-26 | 2010-07-14 | 桂林理工大学 | Method for preparing high-purity sodium niobate nanometer powder |
| CN101891475A (en) * | 2010-07-08 | 2010-11-24 | 桂林理工大学 | Preparation method of potassium-sodium niobate-potassium-bismuth titanate nano ceramics |
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| CN101514103A (en) * | 2009-04-03 | 2009-08-26 | 西北工业大学 | Method for preparing potassium-sodium niobate-sodium bismuth titanate nano ceramics |
| CN101774642A (en) * | 2010-01-26 | 2010-07-14 | 桂林理工大学 | Method for preparing high-purity sodium niobate nanometer powder |
| CN101891475A (en) * | 2010-07-08 | 2010-11-24 | 桂林理工大学 | Preparation method of potassium-sodium niobate-potassium-bismuth titanate nano ceramics |
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