CN108892506A - A kind of method preparing potassium sodium niobate piezoelectric ceramics and potassium sodium niobate piezoelectric ceramics - Google Patents
A kind of method preparing potassium sodium niobate piezoelectric ceramics and potassium sodium niobate piezoelectric ceramics Download PDFInfo
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- CN108892506A CN108892506A CN201810728303.3A CN201810728303A CN108892506A CN 108892506 A CN108892506 A CN 108892506A CN 201810728303 A CN201810728303 A CN 201810728303A CN 108892506 A CN108892506 A CN 108892506A
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- sodium niobate
- potassium sodium
- piezoelectric ceramics
- niobate piezoelectric
- sintering
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/666—Applying a current during sintering, e.g. plasma sintering [SPS], electrical resistance heating or pulse electric current sintering [PECS]
Abstract
The invention discloses a kind of method for preparing potassium sodium niobate piezoelectric ceramics and potassium sodium niobate piezoelectric ceramics.This method uses electric field-assisted sintering technology, i.e., applies electric field on potassium sodium niobate ceramic green body and be sintered, by increasing electric field strength, sintering temperature can be effectively reduced.Fine and close potassium sodium niobate piezoelectric ceramics is obtained within tens seconds in this way, can be sintered under conditions of 300 DEG C lower than conventional sintering temperature, relative density reaches 96%.The present invention solves the problems, such as during conventional sintering to be difficult to densify caused by potassium, sodium alkali metal volatilization.
Description
The invention belongs to leadless piezoelectric ceramics preparation technical fields, prepare potassium sodium niobate piezoelectric ceramics more particularly to a kind of
Method and potassium sodium niobate piezoelectric ceramics.
Background technique
Potassium-sodium niobate (K0.5Na0.5NbO3, abbreviation KNN) and it is a kind of important leadless piezoelectric ceramics, high with Curie temperature,
The features such as piezoelectricity is strong, easily doping property and stability are good.It, can be wide due to electric properties such as its excellent piezoelectricity, dielectric and photoelectricity
It is applied to the high-tech sectors such as electronics, space flight generally, is used to prepare the electronic components such as sensor, energy converter, reservoir, is one
The kind very good electronic functional material of development prospect.
Under normal conditions, it is difficult to prepare the potassium sodium niobate ceramic of high-compactness using conventional solid sintering process, mainly
There is following both sides reason.First, from KNbO3-NaNbO3Binary phase diagraml can see, two phase line of solid-liquid of KNN is very
Gently, therefore during the sintering process the slightly elevated of temperature is possible to generate a large amount of liquid phase, eventually leads to system ceramics
Sintering warm area is especially narrow, and sintering characteristic is excessively poor；Second, the sintering temperature of KNN ceramics is generally greater than 1000 DEG C, at these elevated temperatures
Alkali metal element Na and K are particularly easy to volatilize.Densified sintering product is outside the pale of civilization in addition to being difficult to, and the volatilization of alkali metal can also make under hot conditions
It obtains in sample and generates impurity phase, to reduce its piezoelectric property.Therefore, in order to prepare the potassium-sodium niobate piezoelectricity of fine and close and pure phase
Ceramics, it is necessary to reduce sintering temperature, shorten sintering sintering time.
Summary of the invention
For the defect and deficiency of existing preparation method, potassium-sodium niobate piezoelectricity pottery is prepared the object of the present invention is to provide a kind of
The method and potassium sodium niobate piezoelectric ceramics of porcelain, this method preparation process is simple, and low energy consumption, is suitable for producing in batches.
To achieve the goals above, the technical solution that the present invention takes includes：
A method of potassium sodium niobate piezoelectric ceramics is prepared, is sintered in potassium sodium niobate ceramic green body and prepares potassium-sodium niobate
During piezoelectric ceramics, apply electric field to potassium sodium niobate ceramic green body.
Optionally, the electric field strength of the electric field is 400~700V/cm.
Optionally, the sintering temperature is 800~1000 DEG C, and sintering time is 20~50s.
Optionally, the sintering temperature is 810~950 DEG C, and sintering time is 27~45s.
Optionally, the sintering temperature of the sintering is to be increased to sintering temperature from room temperature, heating rate is 1~50 DEG C/
min。
Optionally, the potassium sodium niobate piezoelectric ceramics green body, which is placed in sintering furnace, is sintered, by potassium-sodium niobate piezoelectricity
Ceramic body is connect with high voltage power supply.
Optionally, the electric current of the high voltage power supply is 50~100mA.
Optionally, the high voltage power supply is DC power supply or AC power source.
Optionally, platinum filament can be used in the connection of potassium sodium niobate piezoelectric ceramics green body and the high voltage power supply or high temperature resistant is led
Electrical filament.
A kind of potassium sodium niobate piezoelectric ceramics, the potassium sodium niobate piezoelectric ceramics are prepared into using method of the present invention
It arrives.
The method provided by the invention for preparing potassium sodium niobate piezoelectric ceramics, has the following advantages that：
(1) it in this way, fine and close potassium sodium niobate piezoelectric ceramics can be prepared Fast Sintering under cryogenic, burns
Junction temperature reduces nearly 300 DEG C compared with conventional sintering temperature, and sintering time is only tens seconds；
(2) in this way, can effectively inhibit the volatilization of Na, K alkali metal element, to prepare the niobium of pure phase and densification
Sour potassium sodium piezoelectric ceramics；
(3) by control electric field strength, it can control the crystallite dimension of gained potassium sodium niobate piezoelectric ceramics；
(4) this method preparation process is simple, and low energy consumption, being capable of mass production potassium sodium niobate piezoelectric ceramics.
Detailed description of the invention
Fig. 1 is the SEM photograph for applying potassium sodium niobate piezoelectric ceramics prepared by not same electric field in embodiment；
Fig. 2 is the XRD diagram for applying potassium sodium niobate piezoelectric ceramics prepared by not same electric field in embodiment；
Fig. 3 is the SEM photograph for applying PZT piezoelectric ceramics prepared by not same electric field in comparative example；
The present invention is illustrated below in conjunction with specification drawings and specific embodiments.
Specific embodiment
Potassium sodium niobate piezoelectric ceramics is usually prepared using solid sintering technology, but is difficult to realize densification, the invention proposes one
Kind promotes the sintering densification process of potassium sodium niobate piezoelectric ceramics using the method that electric field-assisted is sintered, and this method can be effectively
The sintering activity of potassium sodium niobate ceramic is improved, and the volatilization of Na, K alkali element can be prevented, thus quickly preparation under cryogenic
Fine and close and pure phase potassium sodium niobate piezoelectric ceramics out.
It finds in the course of the research, applies external electrical field, the sintering that can be greatly promoted potassium sodium niobate piezoelectric ceramics causes
Densification process, to realize that low temperature Fast Sintering prepares fine and close potassium sodium niobate piezoelectric ceramics ceramic material.By controlling electric-field strength
Degree can also control the grain size of gained potassium sodium niobate piezoelectric ceramics.
The method that the present invention prepares potassium sodium niobate piezoelectric ceramics is that ceramic body is placed in sintering furnace, will be made pottery by platinum filament
Porcelain billet body and high voltage power supply are connected to apply electric field, then under specific sintering temperature, electric field strength and carrying current
It is sintered, to obtain fine and close potassium sodium niobate piezoelectric ceramics.
Specifically, the method that a kind of low temperature Fast Sintering of the invention prepares fine and close potassium sodium niobate piezoelectric ceramics, including with
Lower step:
1) potassium sodium niobate ceramic green body is placed in sintering furnace, and has been connected ceramic body with high voltage power supply by platinum filament
Come；
2) sintering furnace is started to warm up from room temperature, until furnace temperature is 600~1000 DEG C, soaking time is 2~60s, heating
Rate is 1~50 DEG C/min；
3) in sintering furnace temperature-rise period, electric field, electric field level are applied to potassium sodium niobate ceramic green body by high voltage power supply
For 100~1000V/cm；And being arranged through the carrying current in potassium sodium niobate ceramic green body is 5~500mA；
4) sintering furnace and power supply are closed；
Step 1) mesohigh power supply is direct current or AC power source.
Platinum filament can be replaced with the material of high temperature resistant and conduction in step 1).
The present invention promotes the sintering densification process of potassium sodium niobate piezoelectric ceramics material by extra electric field, realizes low
Temperature (<1000 DEG C) quickly (≤1min) prepare potassium sodium niobate piezoelectric ceramics, overcome the defect and deficiency of existing preparation method, institute
The potassium sodium niobate piezoelectric ceramics relative density of preparation is up to 96%, and is pure phase.This method simple process is suitble to batch metaplasia
It produces.
Below with reference to specific embodiment and Figure of description, the present invention is further described.
Embodiment one：
Firstly, use dry-pressing formed technology by potassium sodium niobate ceramic pressed by powder for biscuit, pressure 120MPa, when pressure maintaining
Between be 120s.Potassium sodium niobate ceramic green body is placed in sintering furnace, is connected green body and DC high-voltage power supply by platinum filament.
Setting electric field strength is 400V/cm, carrying current 100mA, sintering furnace is then begun to warm to 1000 DEG C from room temperature, heating
Rate is 10 DEG C/min, when sintering furnace temperature reaches 950 DEG C, after keeping the temperature 30s, and closing sintering furnace and high voltage power supply.After about 2~5h,
Sintered body furnace cooling takes out sample to room temperature.Fig. 1 (a) is the SEM photograph of prepared potassium sodium niobate piezoelectric ceramics, can be with
, it is evident that gained ceramics are almost fine and close, average grain size is 2.15 μm.
Embodiment two：
Firstly, use dry-pressing formed technology by potassium sodium niobate ceramic pressed by powder for biscuit, pressure 120MPa, when pressure maintaining
Between be 120s.Potassium sodium niobate ceramic green body is placed in sintering furnace, is connected green body and DC high-voltage power supply by platinum filament.
Setting electric field strength is 500V/cm, carrying current 100mA, sintering furnace is then begun to warm to 1000 DEG C from room temperature, heating
Rate is 10 DEG C/min, when sintering furnace temperature reaches 920 DEG C, after keeping the temperature 27s, and closing sintering furnace and high voltage power supply.After about 2~5h,
Sintered body furnace cooling takes out sample to room temperature.Fig. 1 (b) is the SEM photograph of prepared potassium sodium niobate piezoelectric ceramics, can be with
, it is evident that gained ceramics are almost fine and close, average grain size is 1.39 μm.Fig. 2 (a) is prepared potassium-sodium niobate piezoelectricity
The XRD diagram of ceramics, all diffraction maximums correspond to potassium-sodium niobate, illustrate that sample is pure phase potassium-sodium niobate, free from admixture phase.
Embodiment three：
Firstly, use dry-pressing formed technology by potassium sodium niobate ceramic pressed by powder for biscuit, pressure 120MPa, when pressure maintaining
Between be 120s.Potassium sodium niobate ceramic green body is placed in sintering furnace, is connected green body and DC high-voltage power supply by platinum filament.
Setting electric field strength is 600V/cm, carrying current 50mA, sintering furnace is then begun to warm to 1000 DEG C from room temperature, heating
Rate is 10 DEG C/min, when sintering furnace temperature reaches 898 DEG C, after keeping the temperature 45s, and closing sintering furnace and high voltage power supply.After about 2~5h,
Sintered body furnace cooling takes out sample to room temperature.Fig. 1 (c) is the SEM photograph of prepared potassium sodium niobate piezoelectric ceramics, can be with
, it is evident that gained ceramics are almost fine and close, average grain size is 0.48 μm.Fig. 2 (b) is prepared potassium-sodium niobate piezoelectricity
The XRD diagram of ceramics, all diffraction maximums correspond to potassium-sodium niobate, illustrate that sample is pure phase potassium-sodium niobate, free from admixture phase.
Example IV：
Firstly, use dry-pressing formed technology by potassium sodium niobate ceramic pressed by powder for biscuit, pressure 120MPa, when pressure maintaining
Between be 120s.Potassium sodium niobate ceramic green body is placed in sintering furnace, is connected green body and DC high-voltage power supply by platinum filament.
Setting electric field strength is 700V/cm, carrying current 50mA, sintering furnace is then begun to warm to 1000 DEG C from room temperature, heating
Rate is 10 DEG C/min, when sintering furnace temperature reaches 810 DEG C, after keeping the temperature 27s, and closing sintering furnace and high voltage power supply.After about 2~5h,
Sintered body furnace cooling takes out sample to room temperature.Fig. 1 (d) is the SEM photograph of prepared potassium sodium niobate piezoelectric ceramics, can be with
, it is evident that gained ceramics are almost fine and close, average grain size is 2.58 μm.
Comparative example one：
Firstly, PZT ceramic powder (commercially available) is compressed to green body using dry-pressing formed technology, pressure 60MPa, when pressure maintaining
Between be 120s.PZT ceramic body is placed in sintering furnace, is connected green body and DC high-voltage power supply by platinum filament, such as Fig. 1
It is shown.Setting electric field strength is 300~600V/cm, then carrying current 100mA begins to warm to sintering furnace from room temperature
800 DEG C, sintering rate is 10 DEG C/min, when sintering furnace temperature reaches 800 DEG C, after keeping the temperature 30s, and closing sintering furnace and high voltage power supply.
After about 2~5h, sample is taken out in sintered body furnace cooling to room temperature.
It is (a) 300V/cm, (b) 400V/cm, (c) 500V/cm, (d) 600V/cm, the limit that Fig. 3, which is respectively in electric field strength,
Electric current is the SEM photograph of prepared PZT piezoelectric ceramics under 100mA, it can be clearly seen that, gained ceramics are completely fine and close.Meanwhile also
As can be seen that average grain size reduces with the increase of electric field strength.In 300V/cm, 400V/cm, 500V/cm, 600V/
Under the electric field strength of cm, average grain size is respectively 3.97 μm, 2.83 μm, 1.89 μm, 1.68 μm.
Claims (10)
1. a kind of method for preparing potassium sodium niobate piezoelectric ceramics, which is characterized in that be sintered system in potassium sodium niobate ceramic green body
During standby potassium sodium niobate piezoelectric ceramics, apply electric field to potassium sodium niobate ceramic green body.
2. the method according to claim 1 for preparing potassium sodium niobate piezoelectric ceramics, which is characterized in that the electricity of the electric field
Field intensity is 400~700V/cm.
3. the method according to claim 1 or 2 for preparing potassium sodium niobate piezoelectric ceramics, which is characterized in that the sintering
Temperature is 800~1000 DEG C, and sintering time is 20~50s.
4. the method according to claim 1 or 2 for preparing potassium sodium niobate piezoelectric ceramics, which is characterized in that the sintering
Temperature is 810~950 DEG C, and sintering time is 27~45s.
5. the method according to claim 1 or 2 for preparing potassium sodium niobate piezoelectric ceramics, which is characterized in that the sintering
Sintering temperature be to be increased to sintering temperature from room temperature, heating rate is 1~50 DEG C/min.
6. the method according to claim 1 or 2 for preparing potassium sodium niobate piezoelectric ceramics, which is characterized in that the niobic acid
Potassium sodium piezoelectric ceramics green body, which is placed in sintering furnace, to be sintered, and potassium sodium niobate piezoelectric ceramics green body is connect with high voltage power supply.
7. the method for preparing potassium sodium niobate piezoelectric ceramics as claimed in claim 6, which is characterized in that the high voltage power supply
Electric current is 50~100mA.
8. the method for preparing potassium sodium niobate piezoelectric ceramics as claimed in claim 6, which is characterized in that the high voltage power supply is
DC power supply or AC power source.
9. the method for preparing potassium sodium niobate piezoelectric ceramics as claimed in claim 6, which is characterized in that the potassium-sodium niobate pressure
Platinum filament or high temperature resistant conductive filament can be used in the connection of electroceramics green body and high voltage power supply.
10. a kind of potassium sodium niobate piezoelectric ceramics, which is characterized in that the potassium sodium niobate piezoelectric ceramics uses claim 1-9
Method described in any claim is prepared.
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Cited By (1)
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| CN110294629A (en) * | 2019-08-15 | 2019-10-01 | 内蒙古科技大学 | A kind of chromic lanthanum ceramics and preparation method thereof |
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Application publication date: 20181127 |