CN104150535B - A kind of method of synthesizing big L/D ratio flaky sodium niobate powder - Google Patents

A kind of method of synthesizing big L/D ratio flaky sodium niobate powder Download PDF

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CN104150535B
CN104150535B CN201410244828.1A CN201410244828A CN104150535B CN 104150535 B CN104150535 B CN 104150535B CN 201410244828 A CN201410244828 A CN 201410244828A CN 104150535 B CN104150535 B CN 104150535B
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sodium niobate
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flaky sodium
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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 kind of method of synthesizing big L/D ratio flaky sodium niobate powder, adopt following steps: with Bi 2o 3, alkaline carbonate and Nb 2o 5for raw material, NaCl is fused salt, prepares sheet Bi by molten-salt growth method 2.5na 3.5nb 5o 18powder, is then placed in nylon barreling tank, adds zirconia ball and dehydrated alcohol carries out barreling, then carries out pre-burning with NaCl fused salt, is incubated after being then warming up to synthesis temperature, obtained containing NaNbO after cooling 3powder mixture; What finally cleaning obtained contains NaNbO 3powder mixture obtain big L/D ratio flaky sodium niobate powder.Compared to Na 2cO 3for the template that raw material is obtained, more evenly, size is larger, and thickness is thinner, and mainly for the preparation of leadless piezoelectric structured pottery, the template of big L/D ratio is more conducive to improving ceramic texture degree and piezoelectric property, significant to the research promoting leadless piezoelectric ceramics.

Description

A kind of method of synthesizing 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 synthesizing big L/D ratio flaky sodium niobate powder.
Background technology
Along with the enhancing of people's environmental consciousness, leadless piezoelectric ceramics receives to be paid close attention to widely and studies.But remain lead base piezoelectric ceramics in widespread use and electronics science and electronic product.Therefore the piezoelectric property how improving leadless piezoelectric ceramics is the key point of problem.
Grain orientation textured is a kind of effective ways improving piezoelectric property.One of gordian technique of the method prepares the sheet mould material of big L/D ratio.Sodium columbate NaNbO 3crystal is because having perovskite structure, and stable chemical nature, can orientation, becomes the ideal chose of mould material.Present sheet NaNbO 3the preparation method of template is a lot, compares and common are single step molten-salt growth method and two step molten-salt growth methods, as the NaNbO that A.Kikuchihara adopts single step molten-salt growth method to prepare 3template, size is at about 10 μm, but thickness reaches 5 μm.(AnnaKikuchiharaandToshioKimura.Microstructuredevelopment in<001>-Oriented (K, Na) NbO 3-basedceramics.Ferroelectrics, 449:102-115,2013); The NaNbO that YasuyoshiSaito adopts topochemistry legal system standby 3template, thickness is about 1 μm, but width average only has 7 μm.(YasuyoshiSaitoandHisaskiTakao.Synthesisofpolycrystalline platelikeNaNbO 3particlesbythetopochemicalmicro-crystalconversionfromK 4nb 6o 17andfabricationofgrain-oriented (K 0.5na 0.5) NbO 3ceramics.JELECTROCERAM, 24:39-45,2010); MingheCao adopts two step molten-salt growth methods, with Na 2cO 3for raw material, the NaNbO of synthesis 3template mean sizes 10 μm, thickness reaches 4tm.(MingheCao，WanqiangWangandFanLi.StructurecontrolofNaNbO 3templatefortexturedceramicsynthesizedbyTwo-stepmoltensaltmethod.Ferroelectrics，404：39-44，2010)。But be all difficult to prepare thin and length-to-diameter ratio is large sheet structure, constrain the application of piezoelectric structured ceramic aspect.
Application number be 200910218770.2 Chinese patent disclose a kind of preparation method of sodium niobate powder: with Nb 2o 5be raw material with NaOH, KOH is mineralizer or with Nb 2o 5for raw material, NaOH is mineralizer, when with Nb 2o 5be raw material with NaOH, 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; The each raw material weighed is added in beaker respectively; Stirring with glass stick makes it dissolve completely; Then through heating, cooling, cleaning and drying process, obtained sodium niobate powder.The powder obtained with the preparation method of this kind of sodium niobate powder is pure rhombic system sodium niobate powder, and adopts the type of heating of microwave " interior heating ", heats more even, improves temperature rise rate, greatly Reaction time shorten.But the sheet size of the sodium niobate powder utilizing the method to prepare about 1 μm, distributes very uneven, constrains the texture degree of piezoelectric ceramics greatly; And employing chemical method, technique is very unstable.
Summary of the invention
Object of the present invention be exactly in order to overcome above-mentioned prior art exist defect and a kind of method that can be used for the synthesis big L/D ratio flaky sodium niobate powder of the kind crystalline substance of template grain growth is provided.
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)
Synthesize a method for big L/D ratio flaky sodium niobate powder, adopt following steps:
(1) with Bi 2o 3, alkaline carbonate and Nb 2o 5for raw material, NaCl is fused salt, prepares sheet Bi by molten-salt growth method 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 carries out barreling, then carries out pre-burning with NaCl fused salt, is incubated after being then warming up to synthesis temperature, obtained containing NaNbO after cooling 3powder mixture;
(3) what cleaning step (2) prepared 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, is warming up to 1000-1100 DEG C of pre-burning 1-4 hour, prepares sheet Bi 805 DEG C of insulations after 1 hour 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 DEG C.
As preferred embodiment, step (3) specifically adopts following steps: first use the deionized water of boiling to soak 24 hours, and constantly change deionized water during the course, then use ultrasonic cleaning, and cleaning is to using AgNO 3after solution inspection washing, solution is without Cl -; And then cleaned product nitric acid is cleaned to solution in acid.
Compared with prior art, the present invention selects three kinds of different carbonate synthesis sames to have the Bi of excellent sheet structure 2.5na 3.5nb 5o 18powder, utilize it under different mol ratio and certain temperature, to obtain highly purified flaky sodium niobate powder as intermediate material carbonate different from three kinds, this flaky sodium niobate powder can be utilized for Template preparation textured ceramic, 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 μm-18 μm, the sheet NaNbO that thickness is 1 μm 3powder, length-to-diameter ratio is (3: 1)-(1.5: 1);
(2) with this sheet NaNbO 3the textured ceramic of powder prepared by template has excellent orientation, greatly improves its piezoelectric property;
(3) prepare skill simple, cost is low, excellent performance, can obtain large length-to-diameter ratio, is mainly used in the preparation of leadless piezoelectric structured pottery, significant to the research promoting leadless piezoelectric ceramics.
(4) molten-salt growth method is adopted successfully to prepare distribution of sizes at 10 μm-18 μm, the sheet NaNbO that thickness is 1 μm 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 chemical constitution to the affecting laws of 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 occupied, Na in fused salt NaCl +radius ratio K +little, replace K in the molten state +, K +washed, generated pure NaNbO 3flaky powder.For casting technique, the NaNbO that we prepare by adopting this method 3sheet template, the piezoelectric property of piezoelectric ceramics is significantly improved, and texture improves 100% compared to non-textured piezoelectric property, and process stabilizing, facilitate the development of piezoelectric ceramics greatly, extend its range of application.
Accompanying drawing explanation
Fig. 1 is with Na 2cO 3for the sheet Bi that raw material is obtained 2.5na 3.5nb 5o 18the SEM figure of powder;
Fig. 2 is with K 2cO 3for the sheet Bi that raw material is obtained 2.5na 3.5nb 5o 18the SEM figure of powder;
Fig. 3 is with K 2cO 3for the sheet Bi that raw material is obtained 2.5na 3.5nb 5o 18the XRD figure spectrum of powder;
Fig. 4 is with Na 2cO 3for the sheet NaNbO that raw material is obtained 3the SEM figure of powder;
Fig. 5 is with K 2cO 3+ Na 2cO 3for the sheet NaNbO that raw material is obtained 3the SEM figure of powder;
Fig. 6 is with K 2cO 3for the sheet NaNbO that raw material is obtained 3the SEM collection of illustrative plates of powder;
Fig. 7 is with K 2cO 3for the sheet NaNbO that raw material is obtained 3the XRD figure spectrum of powder;
Fig. 8 is with K 2cO 3for the sheet NaNbO that raw material is obtained 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 Bi on chip prepared by raw material 2.5na 3.5nb 5o 18powder: take 6.524gBi 2o 3, 1.484gNa 2cO 3and 5.317gNb 2o 5take 14.658gNaCl powder again, all powders are mixed 24 hours with dehydrated alcohol ball milling, mixed material is dried, load alumina crucible put into 805 DEG C, stove insulation 1 hour and heat up (temperature rise rate is 2 DEG C/min) to synthesis temperature 1100 DEG C of pre-burnings 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 3for the sheet Bi that raw material is obtained 2.5na 3.5nb 5o 18the SEM picture of powder, as can be seen from Fig. 1, the Bi of preparation 2.5na 3.5nb 5o 18the particle size range of powder is at 5 μm-20 μm, and thickness 2 μm, size is uneven, and fragment is more.
Embodiment 2
With K 2cO 3for Bi on chip prepared by raw material 2.5na 3.5nb 5o 18powder: take 6.524gBi 2o 3, 1.935gK 2cO 3and 5.317gNb 2o 5take 15.153gNaCl powder again, all powders are mixed 24 hours with dehydrated alcohol ball milling, mixed material is dried, load alumina crucible put into 805 DEG C, stove insulation 1 hour and heat up (temperature rise rate is 2 DEG C/min) to synthesis temperature 1000 DEG C of pre-burnings 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, figure bis-is with K 2cO 3for the sheet Bi that raw material is obtained 2.5na 3.5nb 5o 18the SEM picture of powder, as can be seen from Fig. 2, the Bi of preparation 2.5na 3.5nb 5o 18the particle size range of powder at 15 μm-30 μm, thickness 1 μm.Can clearly find out thus, by K 2cO 3the sheet intermediate product prepared for raw material comparatively with Na 2cO 3for raw material obtains, there is larger length-to-diameter ratio.Fig. 3 is with K 2cO 3for the sheet Bi that raw material is obtained 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 significantly reduces 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, mixed by powder, take dehydrated alcohol as barreling-medium, wherein the quality of zirconia ball is; Barreling 10 hours, loads after discharging drying in alumina crucible, is incubated 2 hours, cools to room temperature with the furnace at 805 DEG C of pre-burnings were warming up to 1000 DEG C after 1 hour.The deionized water of prepared powder boiling is first soaked one day, and constantly changes deionized water, with ultrasonic cleaning, until use AgNO 3after solution inspection washing, solution is without Cl -(removing NaCl).Again cleaned product nitric acid is cleaned repeatedly, (Ex-all Bi till the solution after washing is acidity 2o 3) namely obtain sheet NaNbO 3powder.Fig. 4 is with Na in the present embodiment 2cO 3for the sheet NaNbO that raw material is obtained 3the SEM figure of powder, sheet is very little and uneven 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 optimum 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, mixed by powder, take dehydrated alcohol as barreling-medium, wherein the quality of zirconia ball is 26g; Barreling 10 hours, loads after discharging drying in alumina crucible, is incubated 2 hours, cools to room temperature with the furnace at 805 DEG C of pre-burnings were warming up to 950 DEG C after 1 hour.The deionized water of prepared powder boiling is first soaked one day, and constantly changes deionized water, with ultrasonic cleaning, until use AgNO 3after solution inspection washing, solution is without Cl -(removing NaCl).Again cleaned product nitric acid is cleaned repeatedly, (Ex-all Bi till the solution after washing is acidity 2o 3) namely obtain sheet NaNbO 3powder.Fig. 5 is with Na in the present embodiment 2cO 3+ K 2cO 3for the sheet NaNbO that raw material is obtained 3the SEM figure of powder, NaNbO prepared as seen from the figure 3powder sheet is less, and size is uneven.
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, mixed by powder, take dehydrated alcohol as barreling-medium, wherein the quality of zirconia ball is 10g; Barreling 10 hours, loads after discharging drying in alumina crucible, is incubated 2 hours, cools to room temperature with the furnace at 805 DEG C of pre-burnings were warming up to 900 DEG C after 1 hour.The deionized water of prepared powder boiling is first soaked one day, and constantly changes deionized water, with ultrasonic cleaning, until use AgNO 3after solution inspection washing, solution is without Cl -(removing NaCl).Again cleaned product nitric acid is cleaned repeatedly, (Ex-all Bi till the solution after washing is acidity 2o 3) namely obtain sheet NaNbO 3powder.Fig. 6 is with K in the present embodiment 2cO 3for the sheet NaNbO that raw material is obtained 3the SEM figure of powder, NaNbO prepared as seen from the figure 3powder sheet structure size 10 μm-18 μm, thickness 1 μm, has large length-to-diameter ratio, and distribution uniform.Fig. 7 and Fig. 8 is respectively with K 2cO 3for the sheet NaNbO that raw material is obtained 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 has appearred in <001> direction, is conducive to the growth of textured ceramic.Can find out to only have Na by the EDS power spectrum of Fig. 8, Nb, O exist, and are very pure NaNbO 3powder.
Embodiment 6
Synthesize a method for big L/D ratio flaky sodium niobate powder, adopt following steps:
(1) with Bi 2o 3, Li 2cO 3and Nb 2o 5for raw material, NaCl is fused salt, prepares sheet Bi by molten-salt growth method 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, is warming up to 10001 DEG C of pre-burnings 4 hours, prepares sheet Bi 805 DEG C of insulations after 1 hour 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 carries out barreling, then carries out pre-burning with NaCl fused salt, 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, is incubated after being then warming up to 900 DEG C, obtained containing NaNbO after cooling 3powder mixture;
(3) what cleaning step (2) prepared contains NaNbO 3powder mixture first use the deionized water of boiling to soak 24 hours, and constantly change deionized water during the course, then use ultrasonic cleaning, cleaning is to using AgNO 3after solution inspection washing, solution is without Cl -; And then cleaned product nitric acid is cleaned to solution in acid, i.e. acquisition big L/D ratio flaky sodium niobate powder.
Embodiment 7
Synthesize a method for big L/D ratio flaky sodium niobate powder, adopt following steps:
(1) with Bi 2o 3, K 2cO 3and Nb 2o 5for raw material, NaCl is fused salt, prepares sheet Bi by molten-salt growth method 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 then taking powder total mass 1.5 times is fused salt, is warming up to l100 DEG C of pre-burning l hour, prepares sheet Bi 805 DEG C of insulations after l hour 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 carries out barreling, then carries out pre-burning with NaCl fused salt, 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, is incubated after being then warming up to 1000 DEG C, obtained containing NaNbO after cooling 3powder mixture;
(3) what cleaning step (2) prepared contains NaNbO 3powder mixture first use the deionized water of boiling to soak 24 hours, and constantly change deionized water during the course, then use ultrasonic cleaning, cleaning is to using AgNO 3after solution inspection washing, solution is without Cl -; And then cleaned product nitric acid is cleaned to solution in acid, i.e. acquisition big L/D ratio flaky sodium niobate powder.

Claims (7)

1. synthesize a method for big L/D ratio flaky sodium niobate powder, it 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, prepares sheet Bi by molten-salt growth method 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 carries out barreling, then carries out pre-burning with NaCl fused salt, is incubated after being then warming up to synthesis temperature, obtained containing NaNbO after cooling 3powder mixture;
(3) what cleaning step (2) prepared contains NaNbO 3powder mixture obtain big L/D ratio flaky sodium niobate powder;
Step (1) specifically adopts following steps: by Bi 2o 3, alkaline carbonate and Nb 2o 5be (4-8) in molar ratio: 7:10 proportioning is mixed to get powder, then taking powder total mass 1-1.5 NaCl is doubly fused salt, is warming up to 1000-1100 DEG C of pre-burning 1-4 hour, prepares sheet Bi 805 DEG C of insulations after 1 hour 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.
2. a kind of method of synthesizing 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. a kind of method of synthesizing big L/D ratio flaky sodium niobate powder according to claim 1, is characterized in that, described Na 2cO 3with K 2cO 3mixture in Na 2cO 3with K 2cO 3mol ratio be (1:9)-(5:5).
4. a kind of method of synthesizing 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.
5. a kind of method of synthesizing 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 DEG C.
6. a kind of method of synthesizing 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 deionized water during the course, then use ultrasonic cleaning, cleaning is to using AgNO 3after solution inspection washing, solution is without Cl -; And then cleaned product nitric acid is cleaned to solution in acid.
7. a kind of method of synthesizing 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 prepared 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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