CN105271409A - Preparation method of sheet shaped potassium-sodium niobate powder - Google Patents

Preparation method of sheet shaped potassium-sodium niobate powder Download PDF

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CN105271409A
CN105271409A CN201410359506.1A CN201410359506A CN105271409A CN 105271409 A CN105271409 A CN 105271409A CN 201410359506 A CN201410359506 A CN 201410359506A CN 105271409 A CN105271409 A CN 105271409A
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powder
sheet
nbo
sodium niobate
ball milling
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沈波
李玲玉
白王峰
张杨
翟继卫
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Tongji University
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Tongji University
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Abstract

The invention relates to a preparation method of sheet shaped potassium-sodium niobate powder. The method comprises the following steps: Bi2O3, alkali carbonate and Nb2O5 are raw materials, NaCl is molten salt, and sheet shaped Bi2.5Na3.5Nb5O18 powder is prepared by a molten-salt growth method; then, the sheet shaped Bi2.5Na3.5Nb5O18 powder and alkali carbonate are raw materials, KCl is molten salt, and sheet shaped (K0.5Na0.5)NbO3 powder is prepared by the molten-salt growth method. Compared with the prior art, the preparation method has the advantages of simple process, low cost, high repeatability and good production efficiency; the prepared sheet shaped (K0.5Na0.5)NbO3 powder has a perovskite structure with uniform distribution and large dimension, and can be used as a template of a high draw ratio for preparation of a lead-free piezoelectric textured ceramic, in order to improve texturing degree of the ceramic and the piezoelectric performance; the powder has an important meaning for promoting research of the leadless piezoelectric ceramic.

Description

A kind of sheet potassium-sodium niobate raw powder's production technology
Technical field
The invention belongs to leadless piezoelectric ceramics field, relate to a kind of sheet potassium-sodium niobate raw powder's production technology.
Background technology
Lead base piezoelectric ceramics (PZT), due to its superior piezoelectric property, is widely used in the high-tech such as telecommunications, aviation aspect at present.But PbO accounts for 70% in these plumbum-based materials, this can threaten to HUMAN HEALTH and environment protection, so, seek a kind of leadless piezoelectric ceramics and replace lead base pottery to be a kind of inexorable trend.At present, leadless piezoelectric ceramics system mainly contains BaTiO 3based leadless piezoelectric ceramics, Bi 0.5na 0.5tiO 3based leadless piezoelectric ceramics, base metal niobate based leadless piezoelectric ceramic, tungsten bronze structure leadless piezoelectric ceramics, bismuth laminated leadless piezoelectric ceramic etc.Wherein, base metal niobate based piezoelectric ceramics Curie temperature is high, has anti-ferroelectricity and is subject to people's extensive concern, but compared with traditional lead base piezoelectric ceramics, its piezoelectric property is on the low side, and application cannot replace PZT.Therefore, the piezoelectric property how improving leadless piezoelectric ceramics is the key point solved the problem.
Grain orientation textured is a kind of effective ways improving piezoelectric ceramics piezoelectric property.One of key of the method is exactly prepare mould material, NN (NaNbO 3) be widely used for as mould material, but for KNN [(K 0.5na 0.5) NbO 3] base piezoelectric ceramic, KNN [(K 0.5na 0.5) NbO 3] template is more similar to base-material, can better combine with base-material in curtain coating sintering process, be KNN based leadless piezoelectric ceramics more preferably mould material.Now, the main method of preparation KNN template adopts hydrothermal method, and such as FanZhang etc. adopt hydrothermal method, with Nb 2o 5, KOH and NaOH be raw material, by control K +and Na +ratio, the sheet KNN powder prepared, thickness is about 100nm, width about 1.5 μm, (FanZHANGetal.HydrothermalSynthesisof (K, Na) NbO 3particles.JapaneseJournalofAppliedPhysics, Vol.47, No.9,2008).ShanBai adopts two step hydrothermal methods, the first synthesizing flaky K of the first step 4na 4nb 6o 199H 2o powder, second step is 0.6 μm as Material synthesis thickness, wide is the sheet KNN powder of 7 μm, (ShanBaiandTomoakiKaraki.Two-stepSynthesisofPlatelikePota ssiumSodiumNiobateTemplateParticlesbyHydrothermalMethod. J.Am.Ceram.Soc.96 [8] 2515-2518,2013).Adopt thermochemical method to prepare the sheet KNN powder of gained, sheet distribution of sizes is little, constrains the raising of piezoelectric ceramics texture degree, and thermochemical method efficiency is low, and output is little, is not suitable for producing in enormous quantities, and there is the technical problem of technique instability.
Summary of the invention
Object of the present invention is exactly provide a kind of sheet potassium-sodium niobate raw powder's production technology to overcome defect that above-mentioned prior art exists, and the method is first with Bi 2o 3, K 2cO 3and Nb 2o 5for raw material, NaCl is fused salt, prepares sheet Bi by a molten-salt growth method 2.5na 3.5nb 5o 18powder; Again with sheet Bi 2.5na 3.5nb 5o 18powder, Na 2cO 3for raw material or with sheet Bi 2.5na 3.5nb 5o 18powder, Na 2cO 3and K 2cO 3mixture be raw material, adopt secondary molten-salt growth method to prepare the sheet (K with perovskite structure 0.5na 0.5) NbO 3powder.
Object of the present invention can be achieved through the following technical solutions:
A kind of sheet potassium-sodium niobate raw powder's production technology, the chemical formula of described potassium-sodium niobate is (K 0.5na 0.5) NbO 3, described preparation method is two step molten-salt growth methods, specifically comprises the following steps:
(1) by reaction raw materials Bi 2o 3, K 2cO 3and Nb 2o 5be (4 ~ 8) in molar ratio: be mixed to get powder at 7: 10, adds fused salt to make ball milling material, is placed in nylon ball grinder, then add zirconia ball and dehydrated alcohol, carries out ball milling, dry, high-temperature heat treatment, i.e. obtained sheet Bi 2.5na 3.5nb 5o 18powder;
(2) by sheet Bi obtained for step (1) 2.5na 3.5nb 5o 18powder and alkaline carbonate are 1 in molar ratio: (2.0 ~ 2.5) mix, and add fused salt and make ball milling material, be placed in nylon ball grinder, then add zirconia ball and dehydrated alcohol, carry out ball milling;
(3) by after the batch mixing drying after step (2) ball milling, high-temperature heat treatment is carried out, namely obtained containing (K 0.5na 0.5) NbO 3powder mixture;
(4) what obtain step (3) contains (K 0.5na 0.5) NbO 3powder mixture carry out clean, namely make sheet (K 0.5na 0.5) NbO 3powder.
Fused salt described in step (1) is NaCl, the quality of this fused salt NaCl and described reaction raw materials Bi 20 3, K 2cO 3and Nb 2o 5the ratio of mixed powder total mass is (1 ~ 1.5): 1.
Fused salt described in step (2) is KCl, the quality of this fused salt KCl and described sheet Bi 2.5na 3.5nb 5o 18the ratio of powder and alkaline carbonate mixed powder total mass is (1 ~ 1.2): 1.
The mass ratio of step (1) and the zirconia ball described in step (2) and ball milling material is (1.2 ~ 1.5): 1, the mass ratio of described dehydrated alcohol and ball milling material is (1.5 ~ 3.0): 1, and described Ball-milling Time is 8 ~ 24h.
High-temperature heat treatment condition described in step (1) is 790 ~ 810 DEG C of constant temperature process 1 ~ 2h, then presses ramp to 1000 ~ 1100 DEG C of 1 ~ 3 DEG C/min, after constant temperature process 1 ~ 4h, cools to room temperature with the furnace.
Alkaline carbonate described in step (2) is Li 2cO 3, Na 2cO 3or Na 2cO 3with K 2cO 3be in molar ratio (1 ~ 5): the mixture that (5 ~ 9) form, described alkaline carbonate and sheet Bi 2.5na 3.5nb 5o 18the mol ratio of powder is (1.5 ~ 3.0): 1.
Alkaline carbonate described in step (2) is Na 2cO 3time, itself and sheet Bi 2.5na 3.5nb 5o 18the mol ratio preferred (1.75 ~ 2.5) of powder: 1.
Alkaline carbonate described in step (2) is Na 2cO 3with K 2cO 3during the mixture formed, this mixture and sheet Bi 2.5na 3.5nb 5o 18the mol ratio preferred (2.0 ~ 3.0) of powder: 1.
High-temperature heat treatment condition described in step (3) is 790 ~ 810 DEG C of constant temperature process 1 ~ 2h, then presses ramp to 920 ~ 980 DEG C of 0.5 ~ 1 DEG C/min, after constant temperature process 1 ~ 3h, cools to room temperature with the furnace.
Clean process described in step (4) is: obtained for step (3) is contained (K 0.5na 0.5) NbO 3powder mixture be placed in 100 DEG C of deionized waters, after immersion treatment 12 ~ 24h, then carry out ultrasonic cleaning, until use AgNO 3without Cl in solution after solution inspection washing -, then by cleaned product HNO 3repeatedly clean, till the solution after washing is acidity.
Compared with prior art, the present invention has following characteristics:
(1) (the K that obtains of the present invention 0.5na 0.5) NbO 3the distribution of sizes of powder is 15 μm ~ 25 μm, and thickness is about 1 μm, and dimensional homogeneity is good, Stability Analysis of Structures;
(2) with (K that the present invention obtains 0.5na 0.5) NbO 3the textured ceramic of powder prepared by template, has excellent orientation, can greatly improve its piezoelectric property;
(3) preparation technology is simple, and cost is low, and repeatable strong, production efficiency is high, excellent performance, can obtain the sheet structure that size is large, is mainly used in the preparation of leadless piezoelectric structured pottery, significant to the research promoting leadless piezoelectric ceramics.
Accompanying drawing explanation
Fig. 1 is with K 2cO 3for the sheet Bi that raw material is obtained 2.5na 3.5nb 5o 18the SEM collection of illustrative plates of powder;
Fig. 2 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. 3 is with Na 2cO 3, K 2cO 3the alkaline carbonate of mixing composition and Bi 2.5na 3.5nb 5o 18for the sheet (K that raw material is obtained 0.5na 0.5) NbO 3the SEM collection of illustrative plates of powder;
Fig. 4 is with Na 2cO 3, K 2cO 3the alkaline carbonate of mixing composition and Bi 2.5na 3.5nb 5o 18for the sheet (K that raw material is obtained 0.5na 0.5) NbO 3the EDS collection of illustrative plates of powder;
Fig. 5 is Na 2cO 3with Bi 2.5na 3.5nb 5o 18according to different mol ratio, obtained sheet (K 0.5na 0.5) NbO 3the XRD figure spectrum of powder;
Fig. 6 is with Na 2cO 3with Bi 2.5na 3.5nb 5o 18for raw material, obtained sheet (K 0.5na 0.5) NbO 3the EDS collection of illustrative plates of powder;
Fig. 7 is Bi 2.5na 3.5nb 5o 183with Na 2cO 3be 1: 1.75 according to mol ratio, obtained sheet (K 0.5na 0.5) NbO 3the SEM collection of illustrative plates of powder;
Fig. 8 is Bi 2.5na 3.5nb 5o 183with Na 2cO 3be 1: 2 according to mol ratio, obtained sheet (K 0.5na 0.5) NbO 3the SEM collection of illustrative plates of powder;
Fig. 9 is Bi 2.5na 3.5nb 5o 183with Na 2cO 3be 1: 2.25 according to mol ratio, obtained sheet (K 0.5na 0.5) NbO 3the SEM collection of illustrative plates of powder;
Figure 10 is Bi 2.5na 3.5nb 5o 183with Na 2cO 3be 1: 2.5 according to mol ratio, obtained sheet (K 0.5na 0.5) NbO 3the SEM collection of illustrative plates of powder;
Figure 11 is the sheet (K that the present invention obtains 0.5na 0.5) NbO 3powder and NaNbO 3, KNbO 3xRD figure spectrum.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1:
The present embodiment prepares sheet (K 0.5na 0.5) NbO 3powder, concrete steps are as follows:
(1) by reaction raw materials Bi 2o 3, K 2cO 3and Nb 2o 5be be mixed to get powder, according to NaCl and above-mentioned Bi at 7: 7: 10 in molar ratio 2o 3, K 2cO 3and Nb 2o 5the ratio of mixed powder total mass is 1.1: 1, adds fused salt NaCl and makes ball milling material, be placed in nylon ball grinder; Be 1.2: 1.5: 1 according to the mass ratio of zirconia ball, dehydrated alcohol and ball milling material again, in nylon ball grinder, add zirconia ball and dehydrated alcohol, ball milling mixing 24h, mixed material is dried, loads alumina crucible, be placed in stove, 805 DEG C of process 1h, by the ramp to 1000 DEG C of 2 DEG C/min, after constant temperature process 2h, cool to room temperature with the furnace, again the material after pyroprocessing is put into Büchner funnel, wash away NaCl, dry, be i.e. obtained sheet Bi 2.5na 3.5nb 5o 18powder;
(2) by Na 2cO 3with K 2cO 3be carry out be mixed and made into alkaline carbonate at 1: 1 in molar ratio, the sheet Bi obtained by step (1) 2.5na 3.5nb 5o 18powder and alkaline carbonate are mix obtained powder, according to KCl and above-mentioned sheet Bi at 1: 2 in molar ratio 2.5na 3.5nb 5o 18the ratio of powder, alkaline carbonate mixed powder total mass is 1.1: 1, adds fused salt KCl and makes ball milling material, be placed in nylon ball grinder; Be 1.2: 1.5: 1 according to the mass ratio of zirconia ball, dehydrated alcohol and ball milling material again, in nylon ball grinder, add zirconia ball and dehydrated alcohol, ball milling mixing 10h;
(3) dried by the batch mixing after step (2) ball milling, load alumina crucible, be placed in stove, 790 DEG C of process 1h, by the ramp to 920 DEG C of 0.5 DEG C/min, after constant temperature process 2h, cool to room temperature with the furnace, namely obtained containing (K 0.5na 0.5) NbO 3powder mixture;
(4) obtained for step (3) is contained (K 0.5na 0.5) NbO 3powder mixture be placed in 100 DEG C of deionized waters, after immersion treatment 24h, then carry out ultrasonic cleaning, until use AgNO 3without Cl in solution after solution inspection washing -, then by cleaned product HNO 3repeatedly clean, till the solution after washing is acidity, i.e. obtained sheet (K 0.5na 0.5) NbO 3powder.
As shown in Figure 1, the Bi for preparing of step (1) 2.5na 3.5nb 5o 18powder is sheet, and its particle size range is at 15 μm-30 μm, and thickness is about 1 μm.Fig. 2 is the sheet Bi that step (1) obtains 2.5na 3.5nb 5o 18the XRD figure spectrum of powder, can find out and generate Bi 2.5na 3.5nb 5o 18powder is bismuth laminated.
Fig. 3 is the sheet (K that the present embodiment is made 0.5na 0.5) NbO 3the SEM figure of powder, as seen from Figure 3, (K 0.5na 0.5) NbO 3powder has uniform microtexture, and its particle size range is at 15 μm ~ 25 μm, and thickness is about 1 μm.Fig. 4 is sheet (K obtained in the present embodiment 0.5na 0.5) NbO 3the EDS collection of illustrative plates of powder, the ratio of potassium sodium is suitable, is potassium-sodium niobate material.
Figure 11 shows that obtained (K 0.5na 0.5) NbO 3powder and NaNbO 3, KNbO 3xRD figure spectrum, as shown in Figure 11, (K 0.5na 0.5) NbO 3xRD figure spectrum compared to NaNbO 3offset by about 0.3 ° left, this is due to K +radius is greater than Na +, work as K +replace part Na +form (K 0.5na 0.5) NbO 3time, because ionic radius becomes large, 2 θ angle left avertences are moved, and what this and LeeJSatel before reported is consistent.(LeeJS，JeonJH，ChoiSY.RoleofalkalicarbonateandsaltintopochemicalsynthesisofK 1/2Na 1/2NbO 3andNaNbO 3templates[J].MetalsandMaterialsInternational，2013，19(6)：1283-1287.)。In like manner, (K 0.5na 0.5) NbO 3xRD figure spectrum compared to KNbO 3offset by 0.6 ° to the right, (K 0.5na 0.5) NbO 3xRD figure spectrum peak angle be positioned at KNbO 3and NaNbO 3between.
Embodiment 2:
The present embodiment prepares sheet (K 0.5na 0.5) NbO 3powder, concrete steps are as follows:
(1) by reaction raw materials Bi 2o 3, K 2cO 3and Nb 2o 5be be mixed to get powder, according to NaCl and above-mentioned Bi at 4: 7: 10 in molar ratio 2o 3, K 2cO 3and Nb 2o 5the ratio of mixed powder total mass is 1: 1, adds fused salt NaCl and makes ball milling material, be placed in nylon ball grinder; Be 1.5: 2: 1 according to the mass ratio of zirconia ball, dehydrated alcohol and ball milling material again, in nylon ball grinder, add zirconia ball and dehydrated alcohol, ball milling mixing 12h, mixed material is dried, loads alumina crucible, be placed in stove, 790 DEG C of process 2h, by the ramp to 1100 DEG C of 1 DEG C/min, after constant temperature process 1h, cool to room temperature with the furnace, again the material after pyroprocessing is put into Büchner funnel, wash away NaCl, dry, be i.e. obtained sheet Bi 2.5na 3.5nb 5o 18powder;
(2) by Na 2cO 3with K 2cO 3be carry out be mixed and made into alkaline carbonate at 5: 9 in molar ratio, the sheet Bi obtained by step (1) 2.5na 3.5nb 5o 18powder and alkaline carbonate are mix obtained powder, according to KCl and above-mentioned sheet Bi at 1: 3 in molar ratio 2.5na 3.5nb 5o 18the ratio of powder, alkaline carbonate mixed powder total mass is 1.2: 1, adds fused salt KCl and makes ball milling material, be placed in nylon ball grinder; Be 1.5: 2: 1 according to the mass ratio of zirconia ball, dehydrated alcohol and ball milling material again, in nylon ball grinder, add zirconia ball and dehydrated alcohol, ball milling mixing 12h;
(3) dried by the batch mixing after step (2) ball milling, load alumina crucible, be placed in stove, 810 DEG C of process 2h, by the ramp to 980 DEG C of 1 DEG C/min, after constant temperature process 3h, cool to room temperature with the furnace, namely obtained containing (K 0.5na 0.5) NbO 3powder mixture;
(4) obtained for step (3) is contained (K 0.5na 0.5) NbO 3powder mixture be placed in 100 DEG C of deionized waters, after immersion treatment 24h, then carry out ultrasonic cleaning, until use AgNO 3without Cl in solution after solution inspection washing -, then by cleaned product HNO 3repeatedly clean, till the solution after washing is acidity, i.e. obtained sheet (K 0.5na 0.5) NbO 3powder.
Embodiment 3:
(1) by reaction raw materials Bi 2o 3, K 2cO 3and Nb 2o 5be be mixed to get powder, according to NaCl and above-mentioned Bi at 8: 7: 10 in molar ratio 2o 3, K 2cO 3and Nb 2o 5the ratio of mixed powder total mass is 1.5: 1, adds fused salt NaCl and makes ball milling material, be placed in nylon ball grinder; Be 1.2: 3: 1 according to the mass ratio of zirconia ball, dehydrated alcohol and ball milling material again, in nylon ball grinder, add zirconia ball and dehydrated alcohol, ball milling mixing 8h, mixed material is dried, loads alumina crucible, be placed in stove, 810 DEG C of process 2h, by the ramp to 1100 DEG C of 3 DEG C/min, after constant temperature process 4h, cool to room temperature with the furnace, again the material after pyroprocessing is put into Büchner funnel, wash away NaCl, dry, be i.e. obtained sheet Bi 2.5na 3.5nb 5o 18powder;
(2) by Na 2cO 3with K 2cO 3be carry out be mixed and made into alkaline carbonate at 1: 9 in molar ratio, the sheet Bi obtained by step (1) 2.5na 3.5nb 5o 18powder and alkaline carbonate are mix obtained powder, according to KCl and above-mentioned sheet Bi at 1: 3 in molar ratio 2.5na 3.5nb 5o 18the ratio of powder, alkaline carbonate mixed powder total mass is 1.2: 1, adds fused salt KCl and makes ball milling material, be placed in nylon ball grinder; Be 1.2: 3: 1 according to the mass ratio of zirconia ball, dehydrated alcohol and ball milling material again, in nylon ball grinder, add zirconia ball and dehydrated alcohol, ball milling mixing 8h;
(3) dried by the batch mixing after step (2) ball milling, load alumina crucible, be placed in stove, 810 DEG C of process 2h, by the ramp to 980 DEG C of 0.5 DEG C/min, after constant temperature process 3h, cool to room temperature with the furnace, namely obtained containing (K 0.5na 0.5) NbO 3powder mixture;
(4) obtained for step (3) is contained (K 0.5na 0.5) NbO 3powder mixture be placed in 100 DEG C of deionized waters, after immersion treatment 24h, then carry out ultrasonic cleaning, until use AgNO 3without Cl in solution after solution inspection washing -, then by cleaned product HNO 3repeatedly clean, till the solution after washing is acidity, i.e. obtained sheet (K 0.5na 0.5) NbO 3powder.
Embodiment 4:
The present embodiment prepares sheet (K 0.5na 0.5) NbO 3powder, concrete steps are as follows:
(1) by reaction raw materials Bi 2o 3, K 2cO 3and Nb 2o 5be be mixed to get powder, according to NaCl and above-mentioned Bi at 7: 7: 10 in molar ratio 2o 3, K 2cO 3and Nb 2o 5the ratio of mixed powder total mass is 1.1: 1, adds fused salt NaCl and makes ball milling material, be placed in nylon ball grinder; Be 1.2: 1.5: 1 according to the mass ratio of zirconia ball, dehydrated alcohol and ball milling material again, in nylon ball grinder, add zirconia ball and dehydrated alcohol, ball milling mixing 24h, mixed material is dried, loads alumina crucible, be placed in stove, 805 DEG C of process 1h, by the ramp to 1000 DEG C of 2 DEG C/min, after constant temperature process 2h, cool to room temperature with the furnace, again the material after pyroprocessing is put into Büchner funnel, wash away NaCl, dry, be i.e. obtained sheet Bi 2.5na 3.5nb 5o 18powder;
(2) by sheet Bi obtained for step (1) 2.5na 3.5nb 5o 18powder and alkaline carbonate Na 2cO 3be the obtained powder of 1: 1.75 mixing in molar ratio, according to KCl and above-mentioned sheet Bi 2.5na 3.5nb 5o 18the ratio of powder, alkaline carbonate mixed powder total mass is 1.1: 1, adds fused salt KCl and makes ball milling material, be placed in nylon ball grinder; Be 1.2: 1.5: 1 according to the mass ratio of zirconia ball, dehydrated alcohol and ball milling material again, in nylon ball grinder, add zirconia ball and dehydrated alcohol, ball milling mixing 10h;
(3) dried by the batch mixing after step (2) ball milling, load alumina crucible, be placed in stove, 790 DEG C of process 1h, by the ramp to 920 DEG C of 0.5 DEG C/min, after constant temperature process 2h, cool to room temperature with the furnace, namely obtained containing (K 0.5na 0.5) NbO 3powder mixture;
(4) obtained for step (3) is contained (K 0.5na 0.5) NbO 3powder mixture be placed in 100 DEG C of deionized waters, after immersion treatment 24h, then carry out ultrasonic cleaning, until use AgNO 3without Cl in solution after solution inspection washing -, then by cleaned product HNO 3repeatedly clean, till the solution after washing is acidity, i.e. obtained sheet (K 0.5na 0.5) NbO 3powder.
Embodiment 5:
The present embodiment is at preparation sheet (K 0.5na 0.5) NbO 3in the process of powder, sheet Bi in step (2) 2.5na 3.5nb 5o 18powder and alkaline carbonate Na 2cO 3be the obtained powder of 1: 2 mixing in molar ratio, all the other are with embodiment 4.
Embodiment 6:
The present embodiment is at preparation sheet (K 0.5na 0.5) NbO 3in the process of powder, sheet Bi in step (2) 2.5na 3.5nb 5o 18powder and alkaline carbonate Na 2cO 3be the obtained powder of 1: 2.25 mixing in molar ratio, all the other are with embodiment 4.
Fig. 6 is sheet (K prepared by the present embodiment 0.5na 0.5) NbO 3the EDS power spectrum of powder, can find out from collection of illustrative plates, and the ratio of potassium sodium is consistent, is potassium-sodium niobate material.
Embodiment 7:
The present embodiment is at preparation sheet (K 0.5na 0.5) NbO 3in the process of powder, sheet Bi in step (2) 2.5na 3.5nb 5o 18powder and alkaline carbonate Na 2cO 3be the obtained powder of 1: 2.5 mixing in molar ratio, all the other are with embodiment 4.
Figure 5 shows that in embodiment 5 ~ 7, alkaline carbonate Na 2cO 3with Bi 2.5n a3.5nb 5o 18sheet (the K that powder obtains by different mol ratio 0.5na 0.5) NbO 3the XRD figure spectrum of powder.As seen from Figure 5, as n (Bi 2.5na 3.5nb 5o 18): n (Na 2cO 3)=1: time (2.0 ~ 2.5), (K of generation 0.5na 0.5) NbO 3structure is perovskite structure, has very faint peak during 2 θ=30 °, and being the peak of remaining bismuth oxide, may be because powder does not clean up.This is corresponding with a small amount of Bi content in the EDS power spectrum of Fig. 6.
Fig. 7 ~ 10 are depicted as in embodiment 4 ~ 7, alkaline carbonate Na 2cO 3with Bi 2.5na 3.5nb 5o 18sheet (the K that powder obtains by different mol ratio 0.5na 0.5) NbO 3the SEM collection of illustrative plates of powder, is analyzed by Fig. 7 ~ 10, the sheet (K that embodiment 4 ~ 7 is obtained 0.5na 0.5) NbO 3the size of powder is more or less the same, along with Na 2cO 3the increase of amount, sheet has a little reunion.

Claims (8)

1. a sheet potassium-sodium niobate raw powder's production technology, is characterized in that, the chemical formula of described potassium-sodium niobate is (K 0.5na 0.5) NbO 3, described preparation method is two step molten-salt growth methods, specifically comprises the following steps:
(1) by reaction raw materials Bi 2o 3, K 2cO 3and Nb 2o 5be (4 ~ 8) in molar ratio: be mixed to get powder at 7: 10, adds fused salt to make ball milling material, then add zirconia ball and dehydrated alcohol, carries out ball milling, dry, high-temperature heat treatment, i.e. obtained sheet Bi 2.5na 3.5nb 5o 18powder;
(2) by sheet Bi obtained for step (1) 2.5na 3.5nb 5o 18powder and alkaline carbonate are 1 in molar ratio: (2.0 ~ 2.5) are mixed to get powder, add fused salt and make ball milling material, then add zirconia ball and dehydrated alcohol, carry out ball milling;
(3) by after the batch mixing drying after step (2) ball milling, high-temperature heat treatment is carried out, obtained containing (K 0.5na 0.5) NbO 3powder mixture;
(4) obtained for step (3) is contained (K 0.5na 0.5) NbO 3powder mixture carry out clean, namely make sheet (K 0.5na 0.5) NbO 3powder.
2. a kind of sheet potassium-sodium niobate raw powder's production technology according to claim 1, it is characterized in that, the fused salt described in step (1) is NaCl, the quality of this fused salt NaCl and described reaction raw materials Bi 2o 3, K 2cO 3and Nb 2o 5the ratio of mixed powder total mass is (1 ~ 1.5): 1.
3. a kind of sheet potassium-sodium niobate raw powder's production technology according to claim 1, it is characterized in that, the fused salt described in step (2) is KCl, the quality of this fused salt KCl and described sheet Bi 2.5na 3.5nb 5o 18the ratio of powder and alkaline carbonate mixed powder total mass is (1 ~ 1.2): 1.
4. a kind of sheet potassium-sodium niobate raw powder's production technology according to claim 1, it is characterized in that, the mass ratio of step (1) and the zirconia ball described in step (2) and ball milling material is (1.2 ~ 1.5): 1, the mass ratio of described dehydrated alcohol and ball milling material is (1.5 ~ 3.0): 1, and described Ball-milling Time is 8 ~ 24h.
5. a kind of sheet potassium-sodium niobate raw powder's production technology according to claim 1, it is characterized in that, the condition of the high-temperature heat treatment described in step (1) is 790 ~ 810 DEG C of constant temperature process 1 ~ 2h, again by ramp to 1000 ~ 1100 DEG C of 1 ~ 3 DEG C/min, after constant temperature process 1 ~ 4h, cool to room temperature with the furnace.
6. a kind of sheet potassium-sodium niobate raw powder's production technology according to claim 1, it is characterized in that, the alkaline carbonate described in step (2) is Li 2cO 3, Na 2cO 3or Na 2cO 3with K 2cO 3be in molar ratio (1 ~ 5): the mixture that (5 ~ 9) form, described alkaline carbonate and sheet Bi 2.5na 3.5nb 5o 18the mol ratio of powder is (2.0 ~ 3.0): 1.
7. a kind of sheet potassium-sodium niobate raw powder's production technology according to claim 1, it is characterized in that, high-temperature heat treatment condition described in step (3) is 790 ~ 810 DEG C of constant temperature process 1 ~ 2h, again by ramp to 920 ~ 980 DEG C of 0.5 ~ 1 DEG C/min, after constant temperature process 1 ~ 3h, cool to room temperature with the furnace.
8. a kind of sheet potassium-sodium niobate raw powder's production technology according to claim 1, it is characterized in that, the clean process described in step (4) is: obtained for step (3) is contained (K 0.5na 0.5) NbO 3powder mixture be placed in 100 DEG C of deionized waters, after immersion treatment 12 ~ 24h, then carry out ultrasonic cleaning, until use AgNO 3without Cl in solution after solution inspection washing -, then by cleaned product HNO 3repeatedly clean, till the solution after washing is acidity.
CN201410359506.1A 2014-07-25 2014-07-25 Preparation method of sheet shaped potassium-sodium niobate powder Pending CN105271409A (en)

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CN109553136A (en) * 2018-11-15 2019-04-02 北京工业大学 A method of preparing composite alkali metal niobate powder
CN109553136B (en) * 2018-11-15 2021-03-16 北京工业大学 Method for preparing composite alkali metal niobate powder
CN109734447A (en) * 2019-02-13 2019-05-10 同济大学 Unleaded textured ceramics with excellent temperature stability and preparation method thereof
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CN110342934A (en) * 2019-06-19 2019-10-18 西安交通大学 A kind of micron-stage sheet-like niobic acid sodium crystal and its preparation method and application
CN114538515A (en) * 2022-02-25 2022-05-27 中南大学 Method for preparing single-metal-doped fast-charged niobium oxide material by using melting method

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