CN101186339A - Microwave hydro-thermal synthesis method for sodium niobate potassium niobate leadless piezoelectric ceramic powder - Google Patents

Microwave hydro-thermal synthesis method for sodium niobate potassium niobate leadless piezoelectric ceramic powder Download PDF

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Publication number
CN101186339A
CN101186339A CNA2007101787071A CN200710178707A CN101186339A CN 101186339 A CN101186339 A CN 101186339A CN A2007101787071 A CNA2007101787071 A CN A2007101787071A CN 200710178707 A CN200710178707 A CN 200710178707A CN 101186339 A CN101186339 A CN 101186339A
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ceramic powder
microwave
niobate
piezoelectric ceramic
potassium
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张梅
郭敏
王习东
周媛
张慈
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

The invention relates to a microwave hydrothermal synthesis method for preparation of sodium-potassium and niobate-potassium lead-free piezoelectric ceramic powder, which belongs to the functional material field. The invention is characterized in that: NaOH or KOH solution and Nb2O5 are used as reactants; NaNbO3 or KNbO3 ceramic powder is synthesized by microwave hydrothermal technology; the concentration of NaOH or KOH is 4-8mol/L while the input amount of the Nb2O5 is 0.01 to 0.02 mol; and the reaction temperature is 110 to 150 DEG C and the heat is preserved for 2 to 6 hours. The microwave hydrothermal synthesis method for preparation of sodium-potassium and niobate-potassium lead-free piezoelectric ceramic powder combines the unique heating features of a microwave and the advantage of the hydrothermal method, thus having simple technique, low cost, low consumption and very wide application prospect.

Description

The method of the synthetic sodium niobate potassium niobate leadless piezoelectric ceramic powder of a kind of microwave hydrothermal
Technical field
The invention belongs to field of functional materials, relate to a kind of sodium niobate potassium niobate leadless piezoelectric ceramic powder synthetic method.
Background technology:
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 with the Curie temperature height, have anti-ferroelectricity and be subjected to attracting attention of people.
Sodium columbate, potassium niobate are the dielectric materialss with orthorhombic structure, have anti-ferroelectricity under the room temperature, and antiferroelectric scope is-100～+ 360 ℃, and 0 ℃ with the next ferroelectricity that shows.Through a small amount of Li or the adulterated NaNbO of K 3, KNbO 3Material has strong ferroelectricity, NaNbO more than room temperature 3, KaNbO 3Based leadless piezoelectric ceramics has unique physical properties: low density, high acoustic velocity, specific inductivity, mechanical quality factor and piezoelectric constant span broad etc.All have good performance and application prospects at aspects such as piezoelectricity, pyroelectricity, electric light.Common NaNbO 3Powder is to pass through Nb 2O 5And Na 2CO 3Obtain through solid state reaction is synthetic, the shortcoming of this method is to be difficult to make raw material to mix, and the sintering temperature height of pottery is difficult to the one-component ceramic of synthesis of densified homogeneous.
At present, about the synthetic NaNbO of hydro-thermal 3The research report of powder has, and Vousden is at first Nb 2O 5In NaOH solution, boil synthetic NaNbO 3People such as Kinomura are with Na 8[Nb 6O 19] 13H 2O is a raw material, and NaOH makees mineralizer, uses Hydrothermal Preparation NaNbO 3Human Nb such as Santos 2O 5With the NaOH solution of different concns, at 200 ℃ of NaNbO that synthesize single-phase orthorhombic system 3Powder has been reported differential responses time and different N aOH and Nb 2O 5Mol ratio is to the influence of product.
KNbO 3Adopt traditional solid state sintering mode, sintering temperature height (generally being higher than 1000 ℃), and K 2O has volatility, and high temperature is volatilization easily down, and especially under the sintering atmosphere of humidity, this effect can be more obvious, and the ratio of K and Nb is difficult to control, the KNbO that obtains 3Product purity is low; And high temperature causes growing up unusually of crystal grain, KNbO easily 3Densification relatively the difficulty.Though liquid phase processes such as sol-gel can access pure KNbO 3But, thermal treatment temp very high (generally being higher than 600 ℃), consumes energy height.
The hertzian wave that it is 1m in the 0.1mm scope that microwave typically refers to wavelength, its correspondent frequency scope is 300MHz～300GHz.The essence of microwave action is the effect of hertzian wave to charged particle, be that material adds the polarizability vector that the polarization of interior media under the electromagnetic field effect produces outside and lags behind electric field change and cause the electric current identical with electric field to produce, caused the in-fighting of material, therefore microwave action and its frequency and power density are closely related, also closely related with the dielectric properties of medium.Why microwave can be used in the field of chemical synthesis, is because of having various polar molecules such as water, alcohols, carboxylic-acid in the related reactant of chemical reaction.Under normal conditions, these molecules are rambling kinestate, when microwave oven magnetic gives off the microwave of very high frequency, the micro-wave energy field is with the speed of per second twenty or thirty hundred million times conversion positive-negative polarity constantly, great change has taken place in molecular motion, molecular arrangement is got up and high-speed motion, produce to collide mutually, rub, push, thereby kinetic energy-micro-wave energy is converted into heat energy.Because this kind energy is from reactant solvents inside, itself does not need the medium that conduct heat, and by convection current, sample temperature just can very fast rising, thereby can be comprehensive, and fast, reacting by heating thing solvent reaches the purpose that improves chemical reaction rate equably.Microwave also has non-thermal effect except heat effect is arranged, and can selectively heat, thereby make chemical reaction have certain selectivity.
Microwave hydrothermal is as a kind of new nano materials technology, owing to have the incomparable advantage of the especially traditional synthetic technology of additive method:
(1) microwave heating speed is fast, and the reaction conditions gentleness has been avoided growing up unusually of crystal grain in the material building-up process, can be in the short period of time, and synthetic purity height under the low temperature, fine size, the material that is evenly distributed;
(2) can directly penetrate the sample of certain depth, heat simultaneously at different depths, not need heat transfer process, this body heat effect makes heating fast, evenly;
(3) by regulating the output rating of microwave, the heating state of sample is changed on inertialess ground immediately, be convenient to control automatically and operate continuously;
(4) thermal inertia of microwave heating is little, so sample behind the powered-down, can realize faster cooling in the low temperature environment around; Heat energy utilization rate height (60%～90%), conserve energy greatly.
Therefore, microwave-hydrothermal method prepares nano material high-purity, even particle size distribution and has been subjected to widespread use as a kind of convenient, fast high-efficiency method.
Summary of the invention:
The present invention seeks to advantage, adopt the microwave hydrothermal technology to produce the sodium columbate lead-free piezoelectric ceramic powder in conjunction with hydrothermal method and microwave heating.
The method of the synthetic sodium niobate potassium niobate leadless piezoelectric ceramic powder of a kind of microwave hydrothermal is characterized in that with NaOH or KOH solution, Nb 2O 5Be reactant, adopt the synthetic NaNbO of microwave hydrothermal technology 3Or KNbO 3Ceramic powder, NaOH or KOH concentration are 4-8mol/L, Nb 2O 5Add-on is the 0.01-0.02 mole, and temperature of reaction is 110-150 ℃, and soaking time is 2-6 hour.
The method of the synthetic sodium columbate lead-free piezoelectric ceramic powder of aforesaid microwave hydrothermal, NaOH or KOH optimum concentration range are 5-7mol/L, Nb 2O 5Optimal addn is the 0.013-0.016 mole; The reaction optimum temperature range is 130-140 ℃; Best soaking time is 4-5 hour.
The synthetic sodium niobate potassium niobate leadless piezoelectric ceramic powder of microwave hydrothermal has the heat characteristic of microwave uniqueness and the advantage of hydrothermal method itself simultaneously, and technology is simple, with low cost, less energy-consumption, has very application prospects.
Description of drawings:
Fig. 1: NaNbO 3XRD figure (130 ℃ of temperature of reaction, reaction times 4h)
Fig. 2: KNbO 3XRD figure (130 ℃ of temperature of reaction, time 12h)
Embodiment:
Embodiment 1
Technical process is as follows:
1. configuration concentration is the sodium hydroxide solution of 6mol/L, liquor capacity 60ml;
2. take by weighing 3.75 gram (0.0141mol) Nb 2O 5Powder;
3. with Nb 2O 5Powder with put into the tetrafluoroethylene water heating kettle after potassium hydroxide solution mixes, keep 50% compactedness, stir 1 hour to mixing;
4. water heating kettle is put in the microwave oven, regulated the power knob, control reaction temperature 110-150 ℃, insulation 2-6h.;
Question response fully after, can see liner bottom adularescent precipitation, for detecting the niobate that whether has solubility in the solution, the supernatant liquid in the liner is poured in the beaker dripping hydrochloric acid into to neutral;
6. with deionized water that the white depositions of liner bottom is repeatedly centrifugal to neutral;
7. will be washed till the neutral white depositions, it is dry to put into microwave oven;
8. obtain very pure NaNbO through the XRD test 3Powder.
Embodiment 2
Technical process is as follows:
1. configuration concentration is the potassium hydroxide solution of 6mol/L, liquor capacity 60ml;
2. take by weighing 3.75 gram (O.0141mol) Nb 2O 5Powder;
3. with Nb 2O 5Powder with put into the tetrafluoroethylene water heating kettle after KOH solution mixes, keep 50% compactedness, stir 1 hour to mixing;
4. water heating kettle is put in the microwave oven, regulated the power knob, control reaction temperature 110-150 ℃, insulation 10-24h;
Question response fully after, can see liner bottom adularescent precipitation, for detecting the niobate that whether has solubility in the solution, the supernatant liquid in the liner is poured in the beaker dripping hydrochloric acid into to neutral;
6. with deionized water that the white depositions of liner bottom is repeatedly centrifugal to neutral;
7. will be washed till the neutral white depositions, it is dry to put into microwave oven, obtains powder;
8. obtain very pure KNbO through the XRD test 3Powder
Concrete test-results:
From the mark of XRD figure, see very clearly and under this test conditions, synthesized very pure NaNbO 3Or KNbO 3Powder, and the synthetic NaNbO of the hydro-thermal of comparing 3Or KNbO 3(230 ℃, 24h), microwave hydrothermal has been saved energy to powder, is a kind of new effective route of synthesis.

Claims (2)

1. the method for the synthetic sodium niobate potassium niobate leadless piezoelectric ceramic powder of microwave hydrothermal is characterized in that with NaOH or KOH solution, Nb 2O 5Be reactant, adopt the synthetic NaNbO of microwave hydrothermal technology 3Or KNbO 3Ceramic powder, NaOH or KOH concentration are 4-8mol/L, Nb 2O 5Add-on is the 0.01-0.02 mole, and temperature of reaction is 110-150 ℃, and soaking time is 2-6 hour.
2. as the method for the synthetic sodium niobate potassium niobate leadless piezoelectric ceramic powder of claim 1 microwave hydrothermal, it is characterized in that NaOH or KOH concentration range are 5-7mol/L, Nb 2O 5Add-on is the 0.013-0.016 mole; Range of reaction temperature is 130-140 ℃; Soaking time is 4-5 hour.
CNA2007101787071A 2007-12-04 2007-12-04 Microwave hydro-thermal synthesis method for sodium niobate potassium niobate leadless piezoelectric ceramic powder Pending CN101186339A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101935216A (en) * 2010-08-29 2011-01-05 青岛理工大学 Method for preparing lithium niobium titanium microwave medium ceramic powder by using hydrothermal process
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
CN103570068A (en) * 2013-10-17 2014-02-12 陕西科技大学 ZnNb2O6 fiber with niobite structure and preparation method of ZnNb2O6 fiber
CN103864147A (en) * 2012-12-14 2014-06-18 国家纳米科学中心 Potassium niobate powder and preparation method thereof
CN103950979A (en) * 2014-04-30 2014-07-30 安徽理工大学 Simple, efficient and energy-saving preparation method of niobic acid
CN110357630A (en) * 2019-07-04 2019-10-22 中国科学院上海硅酸盐研究所 A kind of unleaded pyroelectric ceramic material of high-performance sodium niobate base and its preparation method and application
CN111969198A (en) * 2020-08-24 2020-11-20 福州大学 Transition metal potassium niobate solid solution potassium ion battery cathode material and preparation process thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101935216A (en) * 2010-08-29 2011-01-05 青岛理工大学 Method for preparing lithium niobium titanium microwave medium ceramic powder by using hydrothermal process
CN101935216B (en) * 2010-08-29 2014-07-30 青岛理工大学 Method for preparing lithium niobium titanium microwave medium ceramic powder by using hydrothermal process
CN103864147A (en) * 2012-12-14 2014-06-18 国家纳米科学中心 Potassium niobate powder and preparation method thereof
CN103864147B (en) * 2012-12-14 2016-03-16 国家纳米科学中心 A kind of potassium niobate powder and preparation method thereof
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
CN103570068A (en) * 2013-10-17 2014-02-12 陕西科技大学 ZnNb2O6 fiber with niobite structure and preparation method of ZnNb2O6 fiber
CN103570068B (en) * 2013-10-17 2015-11-11 陕西科技大学 A kind of niobite structure ZnNb 2o 6fiber and preparation method thereof
CN103950979A (en) * 2014-04-30 2014-07-30 安徽理工大学 Simple, efficient and energy-saving preparation method of niobic acid
CN103950979B (en) * 2014-04-30 2016-11-23 安徽理工大学 Simple and effective energy-conservation niobic acid preparation method
CN110357630A (en) * 2019-07-04 2019-10-22 中国科学院上海硅酸盐研究所 A kind of unleaded pyroelectric ceramic material of high-performance sodium niobate base and its preparation method and application
CN111969198A (en) * 2020-08-24 2020-11-20 福州大学 Transition metal potassium niobate solid solution potassium ion battery cathode material and preparation process thereof

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