CN101327957A - Method for preparing NaNbO3 superfine power under low temperature - Google Patents

Method for preparing NaNbO3 superfine power under low temperature Download PDF

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CN101327957A
CN101327957A CNA2008101504895A CN200810150489A CN101327957A CN 101327957 A CN101327957 A CN 101327957A CN A2008101504895 A CNA2008101504895 A CN A2008101504895A CN 200810150489 A CN200810150489 A CN 200810150489A CN 101327957 A CN101327957 A CN 101327957A
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powder
nanbo
mixture
superfine
superfine powder
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杨海波
林营
王芬
朱建锋
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a preparation method of NaNbO3 superfine powder at low temperature comprising: firstly mixing the reactants Nb2O5 and Na2CO3 powders and charging an incendiary agent urea by a weight ratio of 80%-200% of the mixture powders into the mixture powders; then calcining the mixture for more than 6 hours at 550-750 DEG C in the reactor; finally grinding the calcined product to obtain the NaNbO3 superfine powder. The prepared NaNbO3 superfine powder is submicron and has advantages of small particle size distribution, good crystalline state, light agglomeration, fine grainularity, narrow particle size distribution and good uniformity. The synthesis temperature can be reduced to about 550 DEG C because of the introduction of urea. The preparation method has advantages of simple technical process and device, convenient operation, easily available of the materials, low cost of powder preparation, which is easy to realize industrial production, thereby the method has very strong practicability.

Description

A kind of low temperature prepares NaNbO 3The method of superfine powder
Technical field
The invention belongs to material science, relate to a kind of low temperature and prepare NaNbO 3The method of superfine powder.
Background technology
Piezoelectric ceramics is important high performance ceramic material, and it all is widely used at numerous areas such as microelectronics.Yet piezoelectric ceramics great majority commonly used at present are to contain the lead base pottery, mainly are at Pb-based lanthanumdoped zirconate titanates system (Pb (Ti, Zr) O 3Write a Chinese character in simplified form and make PZT) and on the doping vario-property on the PZT basis.The main component of PZT base pottery is PbO, and PbO is a kind of deleterious material, under sintering temperature, has volatility, except that human body, environment are worked the mischief, the consistence of product piezoelectric parameter and repeatability is reduced.Therefore, from the angle of environment protection and technical development, the lead-free piezoceramic material that seek to substitute PZT is necessary and is one of urgent subject very.Leadless piezoelectric material material mainly divides BaTiO at present 3Based leadless piezoelectric ceramics, BNT based leadless piezoelectric ceramics, bismuth stratiform leadless piezoelectric ceramics, several classes of niobate lead-free piezoelectric ceramics.Wherein base metal niobate is with Curie temperature height, tool anti-ferroelectricity and be subjected to attracting attention of people.Especially NaNbO 3As antiferroelectric, can form the solid solution ceramic of different qualities with the ferroelectrics of multiple structure.Prepare NaNbO at present 3The method of ceramic powder has solid phase method, hydrothermal method, oxyhydroxide precursor process, mechanize alloyage and polymer precursor method etc.The temperature that solid phase method prepares powder is higher than 850 ℃, and the granularity of gained powder is bigger, and activity is lower.Wang Ying etc. are with Nb 2O 5With NaOH be raw material, adopt hydrothermal method, under 12 hours conditions of 200 ℃ of insulations, synthesized the NaNbO of pure phase 3Powder [Wang Ying, Yi Zhiguo, Yang Qunbao, etc. the hydrothermal method study on the synthesis of sodium niobate powder. Journal of Inorganic Materials, 2007,22:247-252].Because Nb 2O 5Be water insoluble and general soda acid equal solvent, thus higher temperature and pressure need be controlled with hydrothermal method, and soaking time is very long, otherwise be difficult to into phase.H.Muthurajan etc. are with Nb 2O 5, HF, Na 2CO 3With ammoniacal liquor be raw material, adopt the oxyhydroxide precursor process, under the condition of 200 ℃ of insulation 6h, prepared the NaNbO of pure phase 3Powder [H.Muthurajan, H.H.Kumar, V.Samuel, U.N.Gupta, V.Ravi.Novel hydroxide precursors to prepare NaNbO 3And KNbO 3.CeramicsInternational, 2008,34:671-673].Though this method can be synthesized the NaNbO of pure phase at a lower temperature 3Powder, but its technology is complicated, and the degree of crystallinity of synthetic powder is relatively poor, and powder granularity is inhomogeneous.T.Rojac etc. are with Nb 2O 5And Na 2CO 3With ammoniacal liquor be raw material, adopt the mechanize alloyage, under the condition more than the ball milling 20h, prepared the NaNbO of pure phase 3Powder [T.Rojac, O.Massonb, R.Guinebretiere, et al.A study of the mechanochemical synthesis of NaNbO3, Journal of the European Ceramic Society, 2007,27:2265-2271].This method needs long-time ball milling to synthesize, and required energy consumption height because rotating speed is very high, is introduced the trace impurity of ball-milling medium easily.And this method is higher to equipment requirements.Yang Haibos etc. are with Nb 2O 5, Na 2CO 3, citric acid and ethylene glycol is raw material, adopts the polymer precursor method, at 600 ℃ of NaNbO that synthesized pure phase down under the insulation 2h conditions 3Powder [Yang Haibo, woods battalion, Wang Fen, Luo Hongjie. the synthetic and morphology control of the low temperature of sodium columbate submicron powder. Wuhan University of Technology's journal, 2007,29:58-62].Adopt the higher and technology more complicated of this method synthesis temperature, the particle diameter of powder is closely related with thermal treatment process, the low NaNbO that can not obtain pure phase of temperature 3Powder, the high powder reuniting of temperature is more serious, influences powder characteristic.
Summary of the invention
The object of the present invention is to provide a kind of low temperature to prepare NaNbO 3The method of superfine powder, it is simple that this method has technology, low for equipment requirements, and synthesis temperature is low, and energy consumption is low, and desired raw material is cheap, is convenient to advantages such as suitability for industrialized production.
For achieving the above object, the technical solution used in the present invention is:
1) at first, presses chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 80%～200% then in mixed powder;
2) secondly, mixture is put into container, calcining is more than 6 hours in 550 ℃～750 ℃;
3) last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
Invent prepared NaNbO 3Powder is a submicron order, and size-grade distribution is little, and crystalline state is better, and it is light to reunite, fine size, and narrow particle size distribution, characteristics such as homogeneity is good, simultaneously, the urea introducing can reduce synthesis temperature; Synthesis temperature can be reduced to about 550 ℃, and technical process and equipment are simple, and is easy to operate, and raw material cheaply is easy to get, and the powder preparing cost is low, is convenient to realize suitability for industrialized production, and therefore, this method has very strong practicality.
Description of drawings
Fig. 1 is that the mass ratio of reactant and urea is 1: 1 o'clock, 550 ℃ of XRD figure that are incubated 6h gained powder down, and X-coordinate is 2 θ angles among the figure, and unit is " degree ", and ordinate zou is a diffracted intensity, and unit is " cps "
Fig. 2 is that the mass ratio of reactant and urea is 1: 1 o'clock, 600 ℃ of SEM figure that are incubated 6h gained powder down;
Fig. 3 is that the mass ratio of reactant and urea is 1: 1.2 o'clock, 550 ℃ of SEM figure that are incubated 6h gained powder down;
Fig. 4 is that the mass ratio of reactant and urea is 1: 1 o'clock, 700 ℃ of SEM figure that are incubated 6h gained powder down.
Embodiment
Embodiment 1: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 100% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 550 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.As seen from Figure 1, the crystalline structure of gained powder is NaNbO 3
Embodiment 2: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 100% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 600 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.As seen from Figure 2, the granularity of synthetic powder is less, and it is less to distribute, between 1～3 μ m.Crystal grain is grown better, and it is lighter to reunite.
Embodiment 3: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 120% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 550 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.As seen from Figure 3, the granularity of synthetic powder is less, and it is less to distribute, between 1～2 μ m.Crystal grain is grown better, and it is lighter to reunite.
Embodiment 4: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 100% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 700 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.As seen from the figure, the granularity of synthetic powder is less, and it is less to distribute, between 1～4 μ m.Crystal grain is grown better, and it is lighter to reunite.
Embodiment 5: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 200% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 630 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
Embodiment 6: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 150% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 670 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
Embodiment 7: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 180% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 750 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
Embodiment 8: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 80% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 720 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
It is good that the prepared powder of the present invention has a crystal grain development degree, fine size, and the characteristics such as it is light to reunite, Simultaneously, the introducing of incendiary agent can reduce synthesis temperature; Technological process and equipment are simple, and is easy to operate, Raw material cheaply is easy to get, and preparation cost is low, is convenient to suitability for industrialized production.

Claims (9)

1, a kind of low temperature prepares NaNbO 3The method of superfine powder is characterized in that:
1) at first, presses chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 80%～200% then in mixed powder;
2) secondly, mixture is put into container, calcining is more than 6 hours in 550 ℃～750 ℃;
3) last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
2, low temperature according to claim 1 prepares NaNbO 3The method of superfine powder is characterized in that: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 100% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 550 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
3, low temperature according to claim 1 prepares NaNbO 3The method of superfine powder is characterized in that: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 100% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 600 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
4, low temperature according to claim 1 prepares NaNbO 3The method of superfine powder is characterized in that: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 120% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 550 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
5, low temperature according to claim 1 prepares NaNbO 3The method of superfine powder is characterized in that: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 100% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 700 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
6, low temperature according to claim 1 prepares NaNbO 3The method of superfine powder is characterized in that: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 200% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 630 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
7, low temperature according to claim 1 prepares NaNbO 3The method of superfine powder is characterized in that: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 150% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 670 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
8, low temperature according to claim 1 prepares NaNbO 3The method of superfine powder is characterized in that: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 180% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 750 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
9, low temperature according to claim 1 prepares NaNbO 3The method of superfine powder is characterized in that: at first, press chemical formula NaNbO 3With reactant Nb 2O 5And Na 2CO 3Powder mixes, and adds the incendiary material urea of mixed powder quality 80% then in mixed powder; Secondly, mixture is put into container, calcining is more than 6 hours in 720 ℃; At last, with the calcinate porphyrize, promptly obtain NaNbO 3Superfine powder.
CNA2008101504895A 2008-07-29 2008-07-29 Method for preparing NaNbO3 superfine power under low temperature Pending CN101327957A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103381361A (en) * 2013-07-26 2013-11-06 河南大学 Flocculent nanoscale sodium niobate compound photocatalytic material and application thereof in environment purification and hydrogen preparation
CN104016409A (en) * 2014-06-10 2014-09-03 南京航空航天大学 One-step hydro-thermal synthesis method for flaky sodium niobate powder
CN104085922A (en) * 2014-07-14 2014-10-08 湖北大学 Preparation method of high-purity cubic phase sodium niobate nano powder
CN109233829A (en) * 2018-09-14 2019-01-18 广东工业大学 A kind of magnesium erbium ytterbium three mixes sodium niobate and its preparation method and application
CN109467444A (en) * 2018-12-17 2019-03-15 太原理工大学 A kind of sodium niobate column powder and its ceramic preparation method
CN110981479A (en) * 2020-01-10 2020-04-10 陕西科技大学 High-breakdown ferroelectric ceramic and preparation method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103381361A (en) * 2013-07-26 2013-11-06 河南大学 Flocculent nanoscale sodium niobate compound photocatalytic material and application thereof in environment purification and hydrogen preparation
CN103381361B (en) * 2013-07-26 2015-05-06 河南大学 Flocculent nanoscale sodium niobate compound photocatalytic material and application thereof in environment purification and hydrogen preparation
CN104016409A (en) * 2014-06-10 2014-09-03 南京航空航天大学 One-step hydro-thermal synthesis method for flaky sodium niobate powder
CN104085922A (en) * 2014-07-14 2014-10-08 湖北大学 Preparation method of high-purity cubic phase sodium niobate nano powder
CN104085922B (en) * 2014-07-14 2015-12-02 湖北大学 A kind of preparation method of high-purity Emission in Cubic sodium niobate nanometer powder
CN109233829A (en) * 2018-09-14 2019-01-18 广东工业大学 A kind of magnesium erbium ytterbium three mixes sodium niobate and its preparation method and application
CN109233829B (en) * 2018-09-14 2021-09-24 广东工业大学 Magnesium erbium ytterbium three-doped sodium niobate and preparation method and application thereof
CN109467444A (en) * 2018-12-17 2019-03-15 太原理工大学 A kind of sodium niobate column powder and its ceramic preparation method
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

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Open date: 20081224