CN105523760A - Preparation method for sodium columbate ceramic material with stable antiferroelectricity and low dielectric loss - Google Patents

Preparation method for sodium columbate ceramic material with stable antiferroelectricity and low dielectric loss Download PDF

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CN105523760A
CN105523760A CN201510849715.9A CN201510849715A CN105523760A CN 105523760 A CN105523760 A CN 105523760A CN 201510849715 A CN201510849715 A CN 201510849715A CN 105523760 A CN105523760 A CN 105523760A
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侯育冬
朝鲁门
朱满康
郑木鹏
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Beijing University of Technology
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Abstract

The invention provides a preparation method for a sodium columbate ceramic material with stable antiferroelectricity and low dielectric loss, belonging to the field of dielectric ceramic materials. With the method, stability of an antiferroelectric phase in pure sodium columbate ceramic is realized; ferroelectric phase induced by an electric field does not occure in a 100 kv/cm high electric field; and the material has low dielectric loss (less than 2%). The preparation method comprises the following steps: weighing Na2CO3 and Nb2O5 according to a mol stoichiometric ratio of Na to Nb of 1: 1 and putting the two raw materials into a ball milling tank for ball milling, with absolute ethyl alcohol as a ball milling medium; and subjecting powder obtained after batch mixing to dry grinding through a high-energy ball milling method so as to obtain nanometer sodium columbate powder, directly pressurizing and molding the obtained nanometer powder without addition of any binder and then carrying out sintering at 1350 to 1375 DEG C so as to obtain a ceramic body. Determination of a stable antiferroelectric phase is realized through electric performance testing. The preparation method provided by the invention is simple and has low energy consumption. The prepared sodium columbate ceramic material has stable antiferroelectricity and low dielectric loss.

Description

A kind of preparation method of sodium columbate stupalith of low-dielectric loss of stable anti-ferroelectricity
Technical field
The invention belongs to sodium columbate technical field of ceramic material, be specifically related to a kind of preparation method of sodium columbate stupalith of low-dielectric loss of stable anti-ferroelectricity.
Background technology
Sodium columbate (NaNbO 3) be key ingredient in multiple leadless electronic ceramic systems, its pure phase has important application prospect because of antiferroelectric structure in fields such as energy storage capacitor, high-voltage power supply electrical condensers again.Although pure sodium columbate is antiferroelectric phase at ambient temperature in theory, but the sodium columbate pottery adopting conventional ceramic technique to prepare is due to alkali-metal volatilization disappearance, easily there is Lacking oxygen and alkali metal cation room, these rooms form disfigurement model pair, under weak electric field, very easily induce sodium columbate to change (Geetal. by antiferroelectric to ferroelectrics, J.Am.Ceram.Soc., 94,4329 – 4334 (2011)).Thus, the sodium columbate base ceramic systems in bibliographical information is difficult to observe antiferroelectric behavior.In order to obtain stable antiferroelectric phase, the introducing of additional second constituent element stablizer is a kind of important method.The people such as Shimizu and Guo pass through CaZrO 3or SrZrO 3the introducing of the second constituent element reduces system tolerance Summing Factor and improves average electronegativity, and then stable antiferroelectric phase (Shimizuetal., DaltonTrans.44,10763 (2015) andGuoetal., 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 columbate unit phase, the people such as Shimizu apply the volatilization of calcining and sintering process suppression alkali metallic sodium under hypoxic atmosphere, but its result of study still fails to obtain stable antiferroelectric phase (Shimizuetal., J.Am.Ceram.Soc., 97 [6] 1791 – 1796 (2014)).In addition, it should be noted that, obtain practical application, sodium columbate pottery also needs to possess lower dielectric loss (<2%) to suppress components and parts thermal value operationally.
High-energy-milling and powder embedded sintering technique combine by the present invention, sodium niobate nanometer powder is prepared by high-energy ball milling method, realize ball milling and become phase without calcining one step, thus obtain the high-activity nano powder of narrow particle size distribution, and then the volatilization of sodium under high temperature is suppressed by powder embedded sintering method, prepare high-compactness, low defect, the sodium columbate stupalith of low-dielectric loss.Electric performance test proves that acquisition stablizes antiferroelectric polarization behavior, until high-voltage breakdown electric field does not occur antiferroelectric---the transformation of ferroelectric behavior.
Summary of the invention
The object of this invention is to provide a kind of preparation method of sodium columbate pottery of low-dielectric loss of stable anti-ferroelectricity, the material using the method to prepare has high-compactness, low defect, low-dielectric loss (<2%), shows more stable antiferroelectric phase simultaneously.
To achieve these goals, the present invention adopts high-energy ball milling method to prepare sodium niobate nanometer powder.In encloses container, short period of time one step becomes phase at ambient temperature, does not need heat compared with traditional calcining process, can realize the synthesis of narrow size-grade distribution and high-activity nano powder, suppresses the volatilization of alkali metallic sodium in precursor powder preparation process simultaneously.Subsequently; powder embedded sintering technique is adopted to the sintering process of ceramics sample; powder embedded sintering is to doing a protective atmosphere in sintering process; suppress the volatilization of alkali metallic sodium; prevent material from measuring the imbalance of ratio, realize high-compactness, low-dielectric loss; the reliable preparation of stoichiometric ratio sodium columbate pottery, thus the antiferroelectric phase that final acquisition is stable.Volatilization due to sodium in the niobic acid stupalith of usual non-stoichiometric can produce the defects such as Lacking oxygen, and these defects form dipole to the densification hindering ceramic body, and induce antiferroelectric---ferroelectric transformation.
A preparation method for the sodium columbate stupalith of the low-dielectric loss of stable anti-ferroelectricity, is characterized in that, comprise the steps:
(1) by chemical formula NaNbO 3a mole metering take Na than Na:Nb=1:1 2cO 3and Nb 2o 5powder, inserts in ball grinder, and ball milling, after 12 hours, obtains the powder mixed.Due to Na 2cO 3easy water suction, in order to ensure batching metering ratio, Na 2cO 3dry at 200 DEG C before using, and select dehydrated alcohol to be the grinding medium of batch mixing.Na 2cO 3and Nb 2o 5be micron-sized powder.
(2) powder step (1) obtained takes by fixing ratio of grinding media to material and inserts ball milling in high-energy ball milling tank, ball milling condition is: ratio of grinding media to material is 15:1 ~ 30:1, rotational speed of ball-mill 600 ~ 1000/min, Ball-milling Time 30 ~ 120min, obtain the ceramic powder of nanoscale; Its reaction process is as follows:
Na 2CO 3+Nb 2O 5→2NaNbO 3+CO 2↑
Have the particle size of the broken powder of continuous shock due to abrading-ball to be down to nanoscale in the process, the mechanical energy of colliding in addition is constantly passed in powder, thus makes mixed powder, on nanoscale, diffusion reaction occur, and finally completes above-mentioned reaction.
Ball milling condition is preferably: ratio of grinding media to material is 20:1, rotational speed of ball-mill 800/min, and the powder sample obtained during Ball-milling Time 90min becomes phase effect and size dispersity for best, and size-grade distribution is 12 ~ 20nm sodium niobate nanometer powder; Therefore preferred this powder of ball milling is as the ceramic post sintering precursor powder in the present invention.
(3) step (2) is obtained ceramic powder and be directly compressed into base substrate, do not add any binding agent.
(4) base substrate that step (3) obtains is sintered, sintering condition is: the speed of 7 DEG C/min rises to 650 DEG C from room temperature, then the speed of 3.4 DEG C/min rises to 950 DEG C, then the speed of 4 DEG C/min rise to 1350 ~ 1375 DEG C insulation 2 hours after cool to room temperature with the furnace; Simultaneously in sintering process, base substrate is embedded in the powder that step (2) obtains, and sinters.
Above-mentioned materials of the present invention has more stable antiferroelectric phase.Wherein best sample is the ceramics sample that 1365 DEG C of sintering obtain, and its density can reach 98%, room temperature dielectric constant ε r=397, room temperature dielectric loss tan δ=1.3%, meet the requirement of high quality pottery.
Compared with other is invented, the present invention has following remarkable advantage:
(1) the method is by simply mixing low price, the Niobium Pentxoxide being easy to acquisition and sodium carbonate, makes ballmilling energy be transferred in mixed powder at ambient temperature and obtains target powder in the short period of time.This reduces material cost to a great extent, simplifies the complicacy of preparation technology.
(2) in the present invention, high-energy ball milling method is selected to prepare nano-powder.Traditional Method high-temperature calcination is prepared in powder process the volatilization of a part of alkali metallic sodium and the powder granule size that obtains cannot be avoided comparatively large, poor activity; And high-energy ball milling method is the synthesis completing target phase powder at ambient temperature in an airtight container, avoid the volatilization of heating the alkali metallic sodium caused.In addition, nanometer grade powder has higher sintering activity and defect concentration, is conducive to the sintering densification in later stage.In the sintering process in later stage, we take powder embedded sintering method further; buried powder mainly plays the effect of protective atmosphere in sintering process to base substrate; alleviate the volatilization of alkali metallic sodium in base substrate; thus realize high fine and close, the preparation of the sodium columbate pottery of low-dielectric loss (<2%).
(3) the method obtain the T of dielectric properties test data except gaining public acceptance of the sodium columbate ceramics sample of low-dielectric loss cthe Curie peak of=370 DEG C, also obtain about T=100 DEG C one new dielectric peak, this peak was never reported in the existing document of sodium columbate.The appearance at this abnormal dielectric peak illustrates that room temperature has stable antiferroelectric phase to exist, the two ferroelectric hysteresis loop of beam waist type burner of electrical testing display antiferroelectric feature, and test and also not occur antiferroelectric to ferroelectric phase transformation time electric field is added to 100kv/cm, it represents the antiferroelectric stable performance of sodium columbate.
Accompanying drawing explanation
Fig. 1: ratio of grinding media to material is 20:1, rotational speed of ball-mill 800/min, X-ray diffraction (XRD) collection of illustrative plates of the powder sample obtained during Ball-milling Time 90min.
Fig. 2: ratio of grinding media to material is 20:1, rotational speed of ball-mill 800/min, the powder sample accompanying drawing obtained during Ball-milling Time 90min: (a) low multiple transmission electron microscope picture; (b) EDS power spectrum; (c) high multiple transmission electron microscope picture, (d) selected area electron diffraction figure.
Fig. 3: the ceramics sample accompanying drawing that embodiment 2 obtains:
(a) scanning electron microscope (SEM) photograph, (b) grain size distribution figure
Fig. 4: the X ray diffracting spectrum (XRD) of the ceramics sample that embodiment 2 obtains.
Fig. 5: the ceramics sample that embodiment 2 obtains Jie's temperature curve at different frequencies and damage curve.
Fig. 6: the ceramics sample that embodiment 2 obtains P-E loop line at room temperature.
Embodiment
Illustrate substantive distinguishing features of the present invention and remarkable advantage further below by embodiment, but the present invention is not limited to following examples.
Synthesis NaNbO 3precursor powder, this precursor powder adopts Na 2cO 3and Nb 2o 5low price raw material obtains, and its reaction process is as follows: Na 2cO 3+ Nb 2o 5→ 2NaNbO 3+ CO 2↑ (1)
First by Na 2cO 3at 200 DEG C dry 12 hours, subsequently by mol amount than for Na:Nb=1:1 take Na 2cO 3and Nb 2o 5two kinds of raw materials are inserted in ball grinder, batch mixing 12 hours in planetary ball mill; The powder that batch mixing obtains takes by fixing ratio of grinding media to material and inserts ball milling in high-energy ball milling tank, and ball milling condition is: ratio of grinding media to material is 15:1 ~ 20:1, rotational speed of ball-mill 600 ~ 1000/min, Ball-milling Time 30 ~ 120min; The particle size of the broken powder of continuous shock due to abrading-ball is had to be down to nanoscale in the process, separately add the mechanical energy produced in collision to be constantly passed in powder, thus make mixed powder that solid diffusion reaction occur on nanoscale, finally complete reaction in above-mentioned reaction formula (1).Na 2cO 3be easy to water suction, be unfavorable for that the short period of time becomes phase object, therefore select dehydrated alcohol to be the grinding medium of batch mixing.
Na 2cO 3and Nb 2o 5be micron-sized powder.
Embodiment 1:
By ball milling condition be: ratio of grinding media to material is 15:1, rotational speed of ball-mill 1000/min, the NaNbO that during Ball-milling Time 90min, high-energy ball milling prepares 3under powder does not add the prerequisite of any binding agent, directly at the forming under the pressure of 800MPa, diameter is 11.5 millimeters, and thickness is 1.5 millimeter; Then the speed of 7 DEG C/min rises to 650 DEG C from room temperature, and then the speed of 3.4 DEG C/min rises to 950 DEG C, then the speed of 4 DEG C/min rises to 1350 DEG C of powder embedded sinterings, is incubated 2 hours, namely obtains target stupalith.
Embodiment 2:
By ball milling condition be: ratio of grinding media to material is 20:1, rotational speed of ball-mill 800/min, the NaNbO that during Ball-milling Time 90min, high-energy ball milling prepares 3under powder does not add the prerequisite of any binding agent, directly at the forming under the pressure of 800MPa, diameter is 11.5 millimeters, and thickness is 1.5 millimeter; Then the speed of 7 DEG C/min rises to 650 DEG C from room temperature, and then the speed of 3.4 DEG C/min rises to 950 DEG C, then the speed of 4 DEG C/min rises to 1365 DEG C of powder embedded sinterings, is incubated 2 hours, namely obtains target stupalith.Can find out about T=100 DEG C one new dielectric peak from Fig. 5 and 6, this peak was never reported in the existing document of sodium columbate.The appearance at this abnormal dielectric peak illustrates that room temperature has stable antiferroelectric phase to exist, the two ferroelectric hysteresis loop of beam waist type burner of electrical testing display antiferroelectric feature, and test and also not occur antiferroelectric to ferroelectric phase transformation time electric field is added to 100kV/cm, it represents the antiferroelectric stable performance of sodium columbate.
Embodiment 3:
By ball milling condition be: ratio of grinding media to material is 30:1, rotational speed of ball-mill 600/min, the NaNbO that during Ball-milling Time 120min, high-energy ball milling prepares 3under powder does not add the prerequisite of any binding agent, directly at the forming under the pressure of 800MPa, diameter is 11.5 millimeters, and thickness is 1.5 millimeter; Then the speed of 7 DEG C/min rises to 650 DEG C from room temperature, and the speed of 3.4 DEG C/min rises to 950 DEG C, then the speed of 4 DEG C/min rises to 1375 DEG C of powder embedded sinterings, is incubated 2 hours, namely obtains target stupalith.
Comparative example 1:
By ball milling condition be: ratio of grinding media to material is 20:1, rotational speed of ball-mill 800/min, the NaNbO that during Ball-milling Time 90min, high-energy ball milling prepares 3under powder does not add the prerequisite of any binding agent, directly at the forming under the pressure of 800MPa, diameter is 11.5 millimeters, and thickness is 1.5 millimeter; Then the speed of 7 DEG C/min rises to 650 DEG C from room temperature, and then the speed of 3.4 DEG C/min rises to 950 DEG C, then the speed of 4 DEG C/min rises to 1330 DEG C of sintering, is incubated 2 hours, namely obtains target stupalith.
Comparative example 2:
By ball milling condition be: ratio of grinding media to material is 20:1, rotational speed of ball-mill 800/min, the NaNbO that during Ball-milling Time 90min, high-energy ball milling prepares 3under powder does not add the prerequisite of any binding agent, directly at the forming under the pressure of 800MPa, diameter is 11.5 millimeters, and thickness is 1.5 millimeter; Then the speed of 7 DEG C/min rises to 650 DEG C from room temperature, and then the speed of 3.4 DEG C/min rises to 950 DEG C, then the speed of 4 DEG C/min rises to 1380 DEG C of powder embedded sinterings, is incubated 2 hours, namely obtains target stupalith.
Comparative example 3:
By ball milling condition be: ratio of grinding media to material is 30:1, rotational speed of ball-mill 400/min, the NaNbO that during Ball-milling Time 120min, high-energy ball milling prepares 3under powder does not add the prerequisite of any binding agent, directly at the forming under the pressure of 800MPa, diameter is 11.5 millimeters, and thickness is 1.5 millimeter; Then the speed of 7 DEG C/min rises to 650 DEG C from room temperature, and then the speed of 3.4 DEG C/min rises to 950 DEG C, then the speed of 4 DEG C/min rises to 1365 DEG C of sintering, is incubated 2 hours, namely obtains target stupalith.
The correlation performance parameters contrast table of table 1 above-described embodiment and comparative example ceramics sample
Relative density Specific inductivity 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 preparation method for the sodium columbate stupalith of the low-dielectric loss of stable anti-ferroelectricity, is characterized in that, comprise the steps:
(1) by chemical formula NaNbO 3a mole metering take Na than Na:Nb=1:1 2cO 3and Nb 2o 5powder, inserts in ball grinder, and ball milling, after 12 hours, obtains the powder mixed; Na 2cO 3dry at 200 DEG C before using, and select dehydrated alcohol to be the grinding medium of batch mixing; Na 2cO 3and Nb 2o 5be micron-sized powder.
(2) powder step (1) obtained takes by fixing ratio of grinding media to material and inserts ball milling in high-energy ball milling tank, ball milling condition is: ratio of grinding media to material is 15:1 ~ 30:1, rotational speed of ball-mill 600 ~ 1000/min, Ball-milling Time 30 ~ 120min, obtain the ceramic powder of nanoscale; Its reaction process is as follows:
Na 2CO 3+Nb 2O 5→2NaNbO 3+CO 2↑；
(3) step (2) is obtained ceramic powder and be directly compressed into base substrate, do not add any binding agent.
(4) base substrate that step (3) obtains is sintered, sintering condition is: the speed of 7 DEG C/min rises to 650 DEG C from room temperature, then the speed of 3.4 DEG C/min rises to 950 DEG C, then the speed of 4 DEG C/min rise to 1350 ~ 1375 DEG C insulation 2 hours after cool to room temperature with the furnace; Simultaneously in sintering process, base substrate is embedded in the powder that step (2) obtains, and sinters.
2. according to the preparation method of the sodium columbate stupalith of the low-dielectric loss of a kind of stable anti-ferroelectricity according to claim 1, it is characterized in that, step (2) ball milling condition is: ratio of grinding media to material is 20:1, rotational speed of ball-mill 800/min, obtain powder during Ball-milling Time 90min, size-grade distribution is 12 ~ 20nm sodium niobate nanometer powder.
3. according to the preparation method of the sodium columbate stupalith of the low-dielectric loss of a kind of stable anti-ferroelectricity according to claim 1, it is characterized in that, step (4) rises to 1365 DEG C of insulations 2 hours.
4. the sodium columbate stupalith of the low-dielectric loss of the stable anti-ferroelectricity prepared according to the either method of claim 1-3.
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CN115159983A (en) * 2022-07-01 2022-10-11 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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CN107056291A (en) * 2017-04-14 2017-08-18 北京工业大学 A kind of sub-micron crystal yardstick piezoelectric energy collection material and preparation method thereof
CN109809815A (en) * 2019-03-18 2019-05-28 中国科学院上海硅酸盐研究所 A kind of unleaded sodium niobate based antiferroelectric ceramics and preparation method thereof with high saturated polarization and low residual polarization
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
CN110981479A (en) * 2020-01-10 2020-04-10 陕西科技大学 High-breakdown ferroelectric ceramic 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
CN115159983A (en) * 2022-07-01 2022-10-11 中国科学院上海硅酸盐研究所 Sodium niobate-based relaxor antiferroelectric ceramic material 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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