CN104150535A - Method for synthesizing flaky sodium niobate powder with large length-diameter ratio - Google Patents

Method for synthesizing flaky sodium niobate powder with large length-diameter ratio Download PDF

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CN104150535A
CN104150535A CN201410244828.1A CN201410244828A CN104150535A CN 104150535 A CN104150535 A CN 104150535A CN 201410244828 A CN201410244828 A CN 201410244828A CN 104150535 A CN104150535 A CN 104150535A
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sodium niobate
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flaky sodium
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CN104150535B (en
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沈波
李玲玉
白王峰
翟继卫
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Tongji University
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Abstract

The present invention relates to a method for synthesizing flaky sodium niobate powder with a large length-diameter ratio. The method comprises the following steps of preparing flaky Bi2.5Na3.5Nb5O18 powder from Bi2O3, alkali metal carbonate and Nb2O5 as raw materials in the presence of NaCl as molten salt by virtue of a molten-salt growth method, then placing flaky Bi2.5Na3.5Nb5O18 powder into a nylon barreling pot, adding zirconium oxide balls and anhydrous ethanol, barreling and then pre-sintering with NaCl molten salt, raising the temperature to the synthesis temperature, maintaining the temperature and cooling to obtain a powder mixture containing NaNbO3; finally cleaning the powder mixture containing NaNbO3 to obtain flaky sodium niobate powder with the large length-diameter ratio. Compared with a template prepared from Na2CO3 as a raw material, the template prepared from flaky sodium niobate powder disclosed by the invention is more uniform, larger in size and smaller in thickness and mainly used for preparing a lead-free piezoelectric textured ceramic, and the template with a large length-diameter ratio is more conductive to improving the texture degree and piezoelectric properties of the ceramic and is important significance of promoting the research on the lead-free piezoelectric ceramic.

Description

A kind of method of synthetic big L/D ratio flaky sodium niobate powder
Technical field
The invention belongs to leadless piezoelectric ceramics field, especially relate to a kind of method of synthetic big L/D ratio flaky sodium niobate powder.
Background technology
Along with the enhancing of people's environmental consciousness, leadless piezoelectric ceramics has been subject to paying close attention to widely and studying.But remain lead base piezoelectric ceramics in widespread use and electronics science and electronic product.Therefore the piezoelectric property that how to improve leadless piezoelectric ceramics is the key point of problem.
Pottery texturing is a kind of effective ways that improve piezoelectric property.One of gordian technique of the method is to prepare the sheet mould material of big L/D ratio.Sodium columbate NaNbO 3crystal is because having perovskite structure, and stable chemical nature, can be orientated, and becomes the ideal chose of mould material.Present sheet NaNbO 3the preparation method of template is a lot, relatively common are single step molten-salt growth method and two step molten-salt growth methods, the NaNbO that adopts single step molten-salt growth method to prepare as A.Kikuchihara 3template, size is in 10 μ m left and right, but thickness reaches 5 μ m.(Anna Kikuchihara and Toshio Kimura.Microstructure development in<001>-Oriented (K, Na) NbO 3-based ceramics.Ferroelectrics, 449:102-115,2013); Yasuyoshi Saito adopts the standby NaNbO of topochemistry legal system 3template, thickness is about 1 μ m, but width average only has 7 μ m.(Yasuyoshi Saito and Hisaski Takao.Synthesis of polycrystalline platelike NaNbO 3particles by the topochemical micro-crystal conversion from K 4nb 6o 17and fabrication of grain-oriented (K 0.5na 0.5) NbO 3ceramics.J ELECTROCERAM, 24:39-45,2010); Minghe Cao adopts two step molten-salt growth methods, with Na 2cO 3for raw material, synthetic NaNbO 3template mean sizes 10 μ m, thickness reaches 4tm.(Minghe Cao,Wanqiang Wang and Fan Li.Structure control of NaNbO 3template for textured ceramic synthesized by Two-step molten salt method.Ferroelectrics,404:39-44,2010)。But be all difficult to prepare sheet structure thin and that length-to-diameter ratio is large, restricted the application of piezoelectric structured ceramic aspect.
Application number is the preparation method that 200910218770.2 Chinese patent discloses a kind of sodium niobate powder: with Nb 2o 5with NaOH be raw material, KOH is mineralizer or with Nb 2o 5for raw material, NaOH is mineralizer, when with Nb 2o 5with NaOH be raw material, when KOH is mineralizer, take 20-40wt%NaOH, 55-75wt% deionized water, 1-3wt%Nb 2o 5and 2-4wt%KOH; When with Nb 2o 5for raw material, when NaOH is mineralizer, take 20-40wt%NaOH, 55-75wt% deionized water and 1-3wt%Nb2O5; Each raw material weighing is added respectively in beaker; With glass stick, stir it is dissolved completely; Then through heating, cooling, cleaning and drying process, make sodium niobate powder.The powder that the preparation method of this kind of sodium niobate powder of take makes is pure rhombic system sodium niobate powder, and adopts the type of heating of microwave " interior heating ", heat more even, raising temperature rise rate, greatly Reaction time shorten.But, utilize the sheet size 1 μ m left and right of the sodium niobate powder that the method prepares, distribute very inhomogeneous, restricted greatly the texture degree of piezoelectric ceramics; And employing chemical method, technique is very unstable.
Summary of the invention
Object of the present invention is exactly a kind of method that synthetic big L/D ratio flaky sodium niobate powder of the kind crystalline substance that can be used for template grain growth is provided in order to overcome the defect that above-mentioned prior art exists.
Object of the present invention can be achieved through the following technical solutions:
Reaction formula is as follows:
Bi 2O 3+Li 2CO 3/Na 2CO 3/K 2CO 3+Nb 2O 5→Bi 2.5Na 3.5Nb 5O 18+CO 2↑ (1)
Bi 2.5Na 3.5Nb 5O 18+Li 2CO 3/Na 2CO 3/K 2CO 3/(Na 2CO 3+K 2CO 3)→NaNbO 3+Bi 2O 3+CO 2↑ (2)
A method for synthetic big L/D ratio flaky sodium niobate powder, adopts following steps:
(1) with Bi 2o 3, alkaline carbonate and Nb 2o 5for raw material, NaCl is fused salt, by molten-salt growth method, prepares sheet Bi 2.5na 3.5nb 5o 18powder;
(2) by alkaline carbonate and sheet Bi 2.5na 3.5nb 5o 18powder is mixed into ball milling material and is placed in nylon barreling tank, adds zirconia ball and dehydrated alcohol to carry out barreling, then with NaCl fused salt, carries out pre-burning, is incubated after being then warming up to synthesis temperature, makes after cooling and contains NaNbO 3powder mixture;
(3) cleaning step (2) prepares contains NaNbO 3powder mixture obtain big L/D ratio flaky sodium niobate powder.
Alkaline carbonate described in step (1) is Li 2cO 3, Na 2cO 3or K 2cO 3.
As preferred embodiment, step (1) specifically adopts following steps: by Bi 2o 3, alkaline carbonate and Nb 2o 5be (4-8) in molar ratio: 7: 10 proportionings are mixed to get powder, then taking powder total mass 1-1.5 NaCl is doubly fused salt, 805 ℃ of insulations, after 1 hour, is warming up to 1000-1100 ℃ of pre-burning 1-4 hour, prepares sheet Bi 2.5na 3.5nb 5o 18powder.
Alkaline carbonate described in step (2) is Li 2cO 3, Na 2cO 3, K 2cO 3or Na 2cO 3with K 2cO 3mixture.Wherein, Na 2cO 3with K 2cO 3mixture in Na 2cO 3with K 2cO 3mol ratio be (1: 9)-(5: 5).
As preferred embodiment, in step (2), alkaline carbonate and sheet Bi 2.5na 3.5nb 5o 18the mol ratio of powder is (1.4-2.0): 1; The mass ratio of zirconia ball and ball milling material is (1.2-1.5): 1; The mass ratio of dehydrated alcohol and ball milling material is (1.5-3.0): 1.Described synthesis temperature is 900-1000 ℃.
As preferred embodiment, step (3) specifically adopts following steps: first use the deionized water of boiling to soak 24 hours, and constantly change during the course deionized water, then use ultrasonic cleaning, clean to using AgNO 3after solution check washing, solution is without Cl -; And then the product cleaning is cleaned to solution and is acid with nitric acid.
Compared with prior art, the present invention selects the synthetic same of three kinds of different carbonate to have the Bi of excellent sheet structure 2.5na 3.5nb 5o 18powder, utilizes it as intermediate material, to obtain under different moles of proportionings and certain temperature highly purified flaky sodium niobate powder from three kinds of different carbonate, can utilize this flaky sodium niobate powder to prepare textured ceramic for template, and it has following principal feature:
(1) NaNbO of this sheet structure 3the size of powder is with sintering temperature and with carbonate and Bi 2.5na 3.5nb 5o 18mol ratio changes, and can prepare distribution of sizes at 10 μ m-18 μ m, the sheet NaNbO of thickness 1 μ m 3powder, length-to-diameter ratio is (3: 1)-(1.5: 1);
(2) with this sheet NaNbO 3powder is that the prepared textured ceramic of template has excellent orientation, has improved greatly its piezoelectric property;
(3) prepare skill simple, cost is low, and excellent performance can obtain large length-to-diameter ratio, is mainly used in the preparation of leadless piezoelectric structured pottery, significant to promoting the research of leadless piezoelectric ceramics.
(4) adopt molten-salt growth method successfully to prepare distribution of sizes at 10 μ m-18 μ m, the sheet NaNbO of thickness 1 μ m 3powder, the kind that can be used for template grain growth is brilliant, and not only technique is simple, cost is lower, and studies different technique and the affect rule of chemical constitution on its pattern.For bismuth oxide-based layered perovskite structure Bi 2.5na 3.5nb 5o 18, in molten salt react ion process, K +replace Bi 2.5na 3.5nb 5o 18middle Na +the A position occupying, Na in fused salt NaCl +radius ratio K +little, under molten state, replace K +, K +be cleaned, generate pure NaNbO 3flaky powder.For casting technique, we are by the NaNbO that adopts this method to prepare 3sheet template, the piezoelectric property of piezoelectric ceramics is significantly improved, and texture has improved 100% compared to non-texture piezoelectric property, and process stabilizing, has promoted greatly the development of piezoelectric ceramics, has expanded its range of application.
Accompanying drawing explanation
Fig. 1 is with Na 2cO 3the sheet Bi making for raw material 2.5na 3.5nb 5o 18the SEM figure of powder;
Fig. 2 is with K 2cO 3the sheet Bi making for raw material 2.5na 3.5nb 5o 18the SEM figure of powder;
Fig. 3 is with K 2cO 3the sheet Bi making for raw material 2.5na 3.5nb 5o 18the XRD figure spectrum of powder;
Fig. 4 is with Na 2cO 3the sheet NaNbO making for raw material 3the SEM figure of powder;
Fig. 5 is with K 2cO 3+ Na 2cO 3the sheet NaNbO making for raw material 3the SEM figure of powder;
Fig. 6 is with K 2cO 3the sheet NaNbO making for raw material 3the SEM collection of illustrative plates of powder;
Fig. 7 is with K 2cO 3the sheet NaNbO making for raw material 3the XRD figure spectrum of powder;
Fig. 8 is with K 2cO 3the sheet NaNbO making for raw material 3the EDS power spectrum of powder.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
With Na 2cO 3for raw material is prepared Bi on chip 2.5na 3.5nb 5o 18powder: take 6.524gBi 2o 3, 1.484gNa 2cO 3and 5.317gNb 2o 5take again 14.658gNaCl powder, all powders are mixed 24 hours with dehydrated alcohol ball milling, mixed material is dried, pack that alumina crucible is put into the insulation of 805 ℃, stove 1 hour into and heat up (temperature rise rate is 2 ℃/min) to 1100 ℃ of pre-burnings of synthesis temperature 2 hours, cool to room temperature with the furnace, put into Büchner funnel and wash away NaCl, dry and obtain sheet Bi 2.5na 3.5nb 5o 18powder, Fig. 1 is with Na 2cO 3the sheet Bi making for raw material 2.5na 3.5nb 5o 18the SEM picture of powder can be found out in Fig. 1, the Bi of preparation 2.5na 3.5nb 5o 18the particle size range of powder is at 5 μ m-20 μ m, thickness 2 μ m, and size is inhomogeneous, and fragment is more.
Embodiment 2
With K 2cO 3for raw material is prepared Bi on chip 2.5na 3.5nb 5o 18powder: take 6.524gBi 2o 3, 1.935gK 2cO 3and 5.317gNb 2o 5take again 15.153gNaCl powder, all powders are mixed 24 hours with dehydrated alcohol ball milling, mixed material is dried, pack that alumina crucible is put into the insulation of 805 ℃, stove 1 hour into and heat up (temperature rise rate is 2 ℃/min) to 1000 ℃ of pre-burnings of synthesis temperature 2 hours, cool to room temperature with the furnace, put into Büchner funnel and wash away NaCl, dry and obtain sheet Bi 2.5na 3.5nb 5o 18powder, Fig. 2 is with K 2cO 3the sheet Bi making for raw material 2.5na 3.5nb 5o 18the SEM picture of powder can be found out in Fig. 2, the Bi of preparation 2.5na 3.5nb 5o 18the particle size range of powder is at 15 μ m-30 μ m, thickness 1 μ m.Can clearly find out thus, by K 2cO 3the sheet intermediate product of preparing for raw material with Na 2cO 3for making, raw material there is larger length-to-diameter ratio.Fig. 3 is with K 2cO 3the sheet Bi making for raw material 2.5na 3.5nb 5o 18the XRD figure spectrum of powder, that can find out generation is comparatively pure sheet Bi 2.5n a3 .5nb 5o 18powder.And use K 2cO 3for raw material has obviously reduced sintering temperature, more environmental protection, saves.
Embodiment 3
With Na 2cO 3with sheet Bi 2.5na 3.5nb 5o 18powder is raw material, and selection NaCl is fused salt, according to above chemical equation (2), can prepare sheet NaNbO 3powder.Concrete steps are as follows: take 0.541gNa 2cO 3, 3.6gBi 2.5na 3.5nb 5o 18with 4.555gNaCl powder, powder is mixed, take dehydrated alcohol as barreling-medium, wherein the quality of zirconia ball is; Barreling 10 hours, packs in alumina crucible after discharging is dry, 805 ℃ of pre-burnings, after 1 hour, is warming up at 1000 ℃ and is incubated 2 hours, cools to room temperature with the furnace.Prepared powder is first soaked to one day with the deionized water of boiling, and constantly change deionized water, with ultrasonic cleaning, until use AgNO 3after solution check washing, solution is without Cl -(removing NaCl).Again the product cleaning is cleaned repeatedly with nitric acid, until the solution after washing is acidity (Ex-all Bi 2o 3) obtain sheet NaNbO 3powder.Fig. 4 is with Na in the present embodiment 2cO 3the sheet NaNbO making for raw material 3the SEM figure of powder, sheet is very little and inhomogeneous as seen from the figure.
Embodiment 4
With Na 2cO 3+ K 2cO 3with sheet Bi 2.5na 3.5nb 5o 18powder is raw material, and wherein best proportioning is Na 2cO 3: K 2cO 3=7: 3, selection NaCl is fused salt, according to above chemical equation (2), can prepare sheet NaNbO 3powder.Concrete steps are as follows: take 1.190gNa 2cO 3powder, 0.664gK 2cO 3powder, 8.6gBi 2.5na 3.5nb 5o 18powder and 11.5gNaCl powder, mix powder, take dehydrated alcohol as barreling-medium, and wherein the quality of zirconia ball is 26g; Barreling 10 hours, packs in alumina crucible after discharging is dry, 805 ℃ of pre-burnings, after 1 hour, is warming up at 950 ℃ and is incubated 2 hours, cools to room temperature with the furnace.Prepared powder is first soaked to one day with the deionized water of boiling, and constantly change deionized water, with ultrasonic cleaning, until use AgNO 3after solution check washing, solution is without Cl -(removing NaCl).Again the product cleaning is cleaned repeatedly with nitric acid, until the solution after washing is acidity (Ex-all Bi 2o 3) obtain sheet NaNbO 3powder.Fig. 5 is with Na in the present embodiment 2cO 3+ K 2cO 3the sheet NaNbO making for raw material 3the SEM figure of powder, as seen from the figure prepared NaNbO 3powder sheet is less, and size is inhomogeneous.
Embodiment 5
With K 2cO 3with sheet Bi 2.5na 3.5nb 5o 18powder is raw material, and selection NaCl is fused salt, according to above chemical equation (2), can prepare sheet NaNbO 3powder.Concrete steps are as follows: take 0.617gK 2cO 3powder, 3.6gBi 2.5na 3.5nb 5o 18powder and 4.639gNaCl powder, mix powder, take dehydrated alcohol as barreling-medium, and wherein the quality of zirconia ball is 10g; Barreling 10 hours, packs in alumina crucible after discharging is dry, 805 ℃ of pre-burnings, after 1 hour, is warming up at 900 ℃ and is incubated 2 hours, cools to room temperature with the furnace.Prepared powder is first soaked to one day with the deionized water of boiling, and constantly change deionized water, with ultrasonic cleaning, until use AgNO 3after solution check washing, solution is without Cl -(removing NaCl).Again the product cleaning is cleaned repeatedly with nitric acid, until the solution after washing is acidity (Ex-all Bi 2o 3) obtain sheet NaNbO 3powder.Fig. 6 is with K in the present embodiment 2cO 3the sheet NaNbO making for raw material 3the SEM figure of powder, as seen from the figure prepared NaNbO 3powder sheet structure size 10 μ m-18 μ m, thickness 1 μ m, has large length-to-diameter ratio, and distribution uniform.Fig. 7 and Fig. 8 are respectively with K 2cO 3the sheet NaNbO making for raw material 3the XRD figure spectrum of powder and EDS power spectrum, what record as seen from Figure 7 is very complete perovskite structure, and a little texture appearred in <001> direction, is conducive to the growth of textured ceramic.By the EDS power spectrum of Fig. 8, can find out to only have Na, Nb, O exists, and is very pure NaNbO 3powder.
Embodiment 6
A method for synthetic big L/D ratio flaky sodium niobate powder, adopts following steps:
(1) with Bi 2o 3, Li 2cO 3and Nb 2o 5for raw material, NaCl is fused salt, by molten-salt growth method, prepares sheet Bi 2.5na 3.5nb 5o 18powder, specifically adopts following steps: by Bi 2o 3, Li 2cO 3and Nb 2o 5be that 4: 7: 10 proportionings are mixed to get powder in molar ratio, then taking powder total mass l NaCl is doubly fused salt, 805 ℃ of insulations, after 1 hour, is warming up to 10001 ℃ of pre-burnings 4 hours, prepares sheet Bi 2.5na 3.5nb 5o 18powder;
(2) by Li 2cO 3with sheet Bi 2.5na 3.5nb 5o 18powder is mixed into ball milling material and is placed in nylon barreling tank, adds zirconia ball and dehydrated alcohol to carry out barreling, then with NaCl fused salt, carries out pre-burning, wherein, and Li 2cO 3with sheet Bi 2.5na 3.5nb 5o 18the mol ratio of powder is 1.4: 1, and the mass ratio of zirconia ball and ball milling material is 1.2: 1; The mass ratio of dehydrated alcohol and ball milling material is 1.5: 1, be then warming up to 900 ℃ after insulation, make after cooling and contain NaNbO 3powder mixture;
(3) cleaning step (2) prepares contains NaNbO 3powder mixture first use the deionized water of boiling to soak 24 hours, and constantly change during the course deionized water, then use ultrasonic cleaning, clean to using AgNO 3after solution check washing, solution is without Cl -; And then the product cleaning is cleaned to solution and is acid with nitric acid, obtain big L/D ratio flaky sodium niobate powder.
Embodiment 7
A method for synthetic big L/D ratio flaky sodium niobate powder, adopts following steps:
(1) with Bi 2o 3, K 2cO 3and Nb 2o 5for raw material, NaCl is fused salt, by molten-salt growth method, prepares sheet Bi 2.5na 3.5nb 5o 18powder, specifically adopts following steps: by Bi 2o 3, K 2cO 3and Nb 2o 5be that 8: 7: 10 proportionings are mixed to get powder in molar ratio, the NaCl that then takes 1.5 times of powder total masses is fused salt, 805 ℃ of insulations, after l hour, is warming up to l100 ℃ of pre-burning l hour, prepares sheet Bi 2.5na 3.5nb 5o 18powder;
(2) by K 2cO 3with sheet Bi 2.5na 3.5nb 5o l8powder is mixed into ball milling material and is placed in nylon barreling tank, adds zirconia ball and dehydrated alcohol to carry out barreling, then with NaCl fused salt, carries out pre-burning, wherein, and K 2cO 3with sheet Bi 2.5na 3.5nb 5o l8the mol ratio of powder is 2: 1, and the mass ratio of zirconia ball and ball milling material is 1.5: 1; The mass ratio of dehydrated alcohol and ball milling material is 3: l, be then warming up to 1000 ℃ after insulation, make after cooling and contain NaNbO 3powder mixture;
(3) cleaning step (2) prepares contains NaNbO 3powder mixture first use the deionized water of boiling to soak 24 hours, and constantly change during the course deionized water, then use ultrasonic cleaning, clean to using AgNO 3after solution check washing, solution is without Cl -; And then the product cleaning is cleaned to solution and is acid with nitric acid, obtain big L/D ratio flaky sodium niobate powder.

Claims (9)

1. a method for synthetic big L/D ratio flaky sodium niobate powder, is characterized in that, the method adopts following steps:
(1) with Bi 2o 3, alkaline carbonate and Nb 2o 5for raw material, NaCl is fused salt, by molten-salt growth method, prepares sheet Bi 2.5na 3.5nb 5o 18powder;
(2) by alkaline carbonate and sheet Bi 2.5na 3.5nb 5o 18powder is mixed into ball milling material and is placed in nylon barreling tank, adds zirconia ball and dehydrated alcohol to carry out barreling, then with NaCl fused salt, carries out pre-burning, is incubated after being then warming up to synthesis temperature, makes after cooling and contains NaNbO 3powder mixture;
(3) cleaning step (2) prepares contains NaNbO 3powder mixture obtain big L/D ratio flaky sodium niobate powder.
2. the method for a kind of synthetic big L/D ratio flaky sodium niobate powder according to claim 1, is characterized in that, the alkaline carbonate described in step (1) is Li 2cO 3, Na 2cO 3or K 2cO 3.
3. the method for a kind of synthetic big L/D ratio flaky sodium niobate powder according to claim 1 and 2, is characterized in that, step (1) specifically adopts following steps: by Bi 2o 3, alkaline carbonate and Nb 2o 5be (4-8) in molar ratio: 7: 10 proportionings are mixed to get powder, then taking powder total mass 1-1.5 NaCl is doubly fused salt, 805 ℃ of insulations, after 1 hour, is warming up to 1000-1100 ℃ of pre-burning 1-4 hour, prepares sheet Bi 2.5na 3.5nb 5o 18powder.
4. the method for a kind of synthetic big L/D ratio flaky sodium niobate powder according to claim 1, is characterized in that, the alkaline carbonate described in step (2) is Li 2cO 3, Na 2cO 3, K 2cO 3or Na 2cO 3with K 2cO 3mixture.
5. the method for a kind of synthetic big L/D ratio flaky sodium niobate powder according to claim 4, is characterized in that, described Na 2cO 3with K 2cO 3mixture in Na 2cO 3with K 2cO 3mol ratio be (1: 9)-(5: 5).
6. the method for a kind of synthetic big L/D ratio flaky sodium niobate powder according to claim 1, is characterized in that, in step (2),
Alkaline carbonate and sheet Bi 2.5na 3.5nb 5o 18the mol ratio of powder is (1.4-2.0): 1;
The mass ratio of zirconia ball and ball milling material is (1.2-1.5): 1;
The mass ratio of dehydrated alcohol and ball milling material is (1.5-3.0): 1.
7. the method for a kind of synthetic big L/D ratio flaky sodium niobate powder according to claim 1, is characterized in that, the synthesis temperature described in step (2) is 900-1000 ℃.
8. the method for a kind of synthetic big L/D ratio flaky sodium niobate powder according to claim 1, it is characterized in that, step (3) specifically adopts following steps: first use the deionized water of boiling to soak 24 hours, and constantly change during the course deionized water, then use ultrasonic cleaning, clean to using AgNO 3after solution check washing, solution is without Cl -; And then the product cleaning is cleaned to solution and is acid with nitric acid.
9. the method for a kind of synthetic big L/D ratio flaky sodium niobate powder according to claim 1, is characterized in that, the length-to-diameter ratio of the flaky sodium niobate powder preparing is (3: 1)-(1.5: 1).
CN201410244828.1A 2014-06-04 2014-06-04 A kind of method of synthesizing big L/D ratio flaky sodium niobate powder Expired - Fee Related CN104150535B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105986319A (en) * 2015-03-17 2016-10-05 佳能株式会社 Method for manufacturing rectangular parallelepiped-shaped single crystal, rectangular parallelepiped-shaped single crystal, method for manufacturing ceramics, ceramics, piezoelectric element, piezoelectric device, and electronic device
CN109608196A (en) * 2019-01-04 2019-04-12 同济大学 A method of synthesizing of uniform size, good dispersion flaky sodium niobate powder
CN109942995A (en) * 2019-02-01 2019-06-28 哈尔滨理工大学 A kind of sodium niobate/polyvinylidene fluoride composite material of high dielectric property and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
YUNFEI CHANG ET AL.: ""Synthesis and morphology of anisotropic NaNbO3 seed crystals"", 《MATERIALS CHEMISTRY AND PHYSICS》, vol. 111, 31 December 2008 (2008-12-31), pages 195 - 200, XP023180148, DOI: doi:10.1016/j.matchemphys.2008.04.031 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105986319A (en) * 2015-03-17 2016-10-05 佳能株式会社 Method for manufacturing rectangular parallelepiped-shaped single crystal, rectangular parallelepiped-shaped single crystal, method for manufacturing ceramics, ceramics, piezoelectric element, piezoelectric device, and electronic device
US10461241B2 (en) 2015-03-17 2019-10-29 Canon Kabushiki Kaisha Method for manufacturing rectangular parallelepiped-shaped single crystal, rectangular parallelepiped-shaped single crystal, method for manufacturing ceramics, ceramics, piezoelectric element, piezoelectric device, and electronic device
CN109608196A (en) * 2019-01-04 2019-04-12 同济大学 A method of synthesizing of uniform size, good dispersion flaky sodium niobate powder
CN109608196B (en) * 2019-01-04 2021-10-08 同济大学 Method for synthesizing flaky sodium niobate powder with uniform size and good dispersibility
CN109942995A (en) * 2019-02-01 2019-06-28 哈尔滨理工大学 A kind of sodium niobate/polyvinylidene fluoride composite material of high dielectric property and preparation method thereof

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