CN110041073A - A kind of preparation method of potassium sodium niobate ceramic - Google Patents
A kind of preparation method of potassium sodium niobate ceramic Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of potassium sodium niobate ceramic.The preparation method is the following steps are included: will be mainly by nanometer KxNa1‑ xNbO3Powder, niobium source, potassium resource, sodium source and solvent composition mixing abrasive lapping it is uniform after, be pressed into block in the case where temperature is 150-160 DEG C, pressure is 430-440MPa, be dried, be heat-treated later at 700 DEG C or more to get.Solid phase particles are reset in the pressing process of the preparation method, and the point contact position, niobium source between particle occur dissolution with similar natural pattern of metallogeny, reaction, potassium-sodium niobate amorphous substance process are precipitated, and the amorphous substance of precipitation is filled in KxNa1‑xNbO3With interstitial site around particle, inner void is reduced, increases the consistency of material, postmenstruation is heat-treated amorphous substance crystallization, so that particle is gradually become polygon from spherical shape, ultimately form densification polycrystalline structure, is significantly improved the consistency of ceramics and piezoelectric property.
Description
Technical field
The invention belongs to potassium sodium niobate ceramic fields, and in particular to a kind of preparation method of potassium sodium niobate ceramic.
Background technique
Piezoelectric ceramics is a kind of ceramic material that can mutually convert electric energy and mechanical energy, belongs to inorganic non-metallic
One kind of material.From piezoelectric effect discovery since, lead base piezoelectric ceramics (PZT) be market principal item, but in PZT lead content
It is higher, environmental problem can be faced in production and application process.Potassium sodium niobate ceramic is with its feature of environmental protection and more superior piezoelectricity
Performance receives significant attention.
There are sintering temperatures high (1100-1200 DEG C), technique week for the potassium sodium niobate ceramic prepared using conventional sintering technique
The drawback of phase length.There are many technique (such as microwave sintering, discharge plasma sintering, two-step sinterings etc.) to reduce potassium niobate
The sintering temperature of sodium ceramics, but it is still undesirable to the reducing effect of sintering temperature.
Publication No. is that the Chinese invention patent application of CN108585847A discloses a kind of preparation of potassium-sodium niobate-based ceramics
Method, comprising the following steps: prepare K first0.5Na0.5NbO3Then powder takes a certain amount of K0.5Na0.5NbO3It is added in powder
The potassium hydroxide and sodium hydroxide mixed solution of weight 10% are fully ground uniformly, then by the material after grinding in mortar
Apply the compression moulding of 350MPa pressure at 120 DEG C, pressure maintaining 120min obtains green body；Green body obtained is filled at 120 DEG C again
Divide drying to be placed in Muffle furnace sintering processes 240min under the conditions of 650 DEG C of temperature, then cooled to room temperature, is made
Potassium sodium niobate ceramic.Although the preparation method realizes the low-temperature sintering preparation of potassium sodium niobate ceramic, but its consistency and piezoelectricity
Performance still needs to be further increased.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of potassium sodium niobate ceramic, to solve existing sintering method preparation
Potassium sodium niobate ceramic consistency and piezoelectric property need the problem of being further increased.
To achieve the above object, technical solution used by the preparation method of potassium sodium niobate ceramic of the invention is:
A kind of preparation method of potassium sodium niobate ceramic, comprising the following steps: will be mainly by nanometer KxNa1-xNbO3Powder, niobium
After the mixing abrasive lapping that source, potassium resource, sodium source and solvent form is uniform, in the case where temperature is 150-160 DEG C, pressure is 430-440MPa
Be pressed into block, be dried, be heat-treated later at 700 DEG C or more to get；
The niobium source, potassium resource, the dosage of sodium source meet KxNa1-xNbO3Stoichiometric ratio, converted after the heat treatment
It is afterwards KxNa1-xNbO3；KxNa1-xNbO3In, 0 < x < 1.
The preparation method of potassium sodium niobate ceramic provided by the invention, to nanometer KxNa1-xNbO3Powder, niobium source, potassium resource, sodium source
Compacting base is carried out with the half fluidised form mixture of solvent composition, solid phase particles are reset in pressing process, nanometer KxNa1-xNbO3
Point contact position, niobium source between powder granule occur dissolution, reaction with similar natural pattern of metallogeny, potassium-sodium niobate are precipitated without fixed
Shape object process, the amorphous substance of precipitation are filled in KxNa1-xNbO3With interstitial site around particle, inner void is reduced, is increased
The consistency of material, postmenstruation are heat-treated amorphous substance crystallization, so that particle is gradually become polygon from spherical shape, ultimately form densification
Change polycrystalline structure, is significantly improved the consistency of ceramics and piezoelectric property.
In process of lapping, wet with solvent solid particles surface is ready for later period particle by migration of liquid and rearrangement,
Mixture is advisable with half fluidised form, it is preferred that in mixture, the mass content of solvent is not more than 15%.
In pressing process, KxNa1-xNbO3Powder granule is wetted, is suppressed under certain temperature and pressure, and moisture steams
Hair, KxNa1-xNbO3The liquid on powder granule surface reaches hypersaturated state, can be in KxNa1-xNbO3Powder granule surface forms nothing
Amorphous mass (potassium-sodium niobate or its presoma) tends to form quasi- homotype phase boundary in green body, forms densification for subsequent heat treatment
Change polycrystalline structure to be ready.Preferably, the time of compacting is 1-120min.
Mold directly can be heated to 150-160 DEG C in advance, mixture is directly added into and carries out heat-insulation pressure keeping process, heating up
It will appear the volatilization of moisture in (heat preservation) pressing process, this process also further promotes the precipitation of amorphous substance.For into one
Step optimization pressing process, promotes to form consistency and the good green body of uniformity, it is preferred that temperature is 150-160 DEG C, pressure is
Before suppressing under 430-440MPa, 10-15min is suppressed under being first 430-440MPa in room temperature, pressure.
From it is energy saving, promote sufficiently the converting of crystal form, further increase product consistency in terms of comprehensively consider, preferably
, the time of the heat treatment is 3-4h.
For the preparation for being further simplified mixture, make liquid phase to nanometer KxNa1-xNbO3The wetting effect of powder is more preferable, thus
Promote densification polycrystalline structure formation, it is preferred that the mixture is prepared by following steps: first by niobium source, potassium resource,
Sodium source and solvent are configured to suspension, then by KxNa1-xNbO3Powder and the suspension ground and mixed are uniform；The matter of suspension
Amount is nanometer KxNa1-xNbO3The 30-40% of powder quality.
Advanced optimize the dispersing uniformity of mixture, it is preferred that the concentration of potassium resource is 2-10mol/L in suspension.
Specific embodiment
Invention broadly provides a kind of low temperature densification techniques of potassium sodium niobate ceramic, mainly by nanometer KxNa1- xNbO3Powder, niobium source, potassium resource, sodium source and solvent ground and mixed apply certain pressure and temperature at half fluidised form mixture later,
Solid phase particles are reset in pressing process, KxNa1-xNbO3Point contact position, niobium source between powder granule with it is similar naturally at
Mine mode occurs dissolution, reaction, potassium-sodium niobate amorphous substance process is precipitated, and the amorphous substance of precipitation is filled in KxNa1-xNbO3?
Grain surrounding and interstitial site, reduce inner void, increase the consistency of material, and postmenstruation is heat-treated amorphous substance crystallization, makes
Particle gradually becomes polygon from spherical shape, ultimately forms densification polycrystalline structure, and then makes the consistency and piezoelectric property of ceramics
It is significantly improved.
Mixture, which can be used, directly to feed, is fully ground mixing, to reach uniform half fluidised form form.Niobium source, potassium resource, sodium
Source and solvent quality summation are nanometer KxNa1-xNbO3The 30-40% of powder (partial size may be selected to be 50-100nm) quality.Mixture
The content of middle solvent is considerably less, generally below 15wt.%, even < 1wt.%.
Following methods can also be used in the preparation of half fluidised form mixture: first being configured to suspend by niobium source, potassium resource, sodium source and solvent
Liquid, then by nanometer KxNa1-xNbO3Powder and suspension ground and mixed are at half fluidised form mixture.Nb may be selected in niobium source2O5Deng.It is outstanding
Supernatant liquid mode can improve Nb to a certain extent2O5Solubility, also facilitate and KxNa1-xNbO3Each component disperses after powder mixing
Uniformly, the dispersion effect of suspension can further be enhanced in suspension containing cosolvents such as ethyl alcohol.
Ground and mixed can be realized using grinder, it is however generally that, grinding 1-2min at 800r/min can meet the requirements.
Pressing process after ground and mixed under certain temperature and pressure is most important to densification polycrystalline structure is formed, and presses
It will appear the volatilization of moisture during system, this process also further promotes the precipitation of amorphous substance；Moisture in pressing process
Passing away is limited, dry incomplete, and processing need to be further dried to remove residual water.The temperature of drying process can be
110-200 DEG C, the time may be set to 10-14h.
When heat treatment, densification potassium sodium niobate ceramic can be formed by keeping the temperature at least 3h at 700 DEG C or more, from energy saving side
Face considers, it is preferred that the temperature of heat treatment is 700-900 DEG C.Being warming up to 700-900 DEG C of rate may be set to 2-8 DEG C/min.
Embodiments of the present invention are described further combined with specific embodiments below.
The specific embodiment of the preparation method of potassium sodium niobate ceramic of the invention is as follows:
Embodiment 1
The preparation method of the potassium sodium niobate ceramic of the present embodiment, using following steps:
1) Nb is taken2O5, KOH, NaOH and deionized water be configured to suspension, wherein Nb2O5, KOH, NaOH three mole
Than for Nb2O5: KOH:NaOH=1:1:1, the concentration of KOH is 5mol/L in suspension；
2) K for being 100nm by suspension and partial size0.5Na0.5NbO3It is put into mold, suspends after powder ground and mixed 2min
The weight of liquid accounts for K0.5Na0.5NbO3The 30% of powder weight；
3) to the material uniaxial compression 430MPa in mold, it is incubated at room temperature pressure maintaining 13min, then with 9 DEG C/min's
Heating rate is warming up to 160 DEG C, and heat-insulation pressure keeping 30min obtains blank；
4) blank is kept the temperature at 200 DEG C 12h, is warming up to 800 DEG C later with the heating rate of 5 DEG C/min, and keep the temperature
Densification piezoelectric ceramics is made in 3.5h.
Embodiment 2
The preparation method of the potassium sodium niobate ceramic of the present embodiment, using following steps:
1) Nb is taken2O5, KOH, NaOH and deionized water be configured to suspension, wherein Nb2O5, KOH, NaOH three mole
Than for Nb2O5: KOH:NaOH=1:1:1, the concentration of KOH is 2mol/L in suspension；
2) K for being 80nm by suspension and partial size0.5Na0.5NbO3It is put into mold, suspends after powder ground and mixed 1min
The weight of liquid accounts for K0.5Na0.5NbO3The 35% of powder weight；
3) to the material uniaxial compression 430MPa in mold, it is incubated at room temperature pressure maintaining 12min, then with 9 DEG C/min's
Heating rate is warming up to 158 DEG C, and heat-insulation pressure keeping 1min obtains blank；
4) blank is kept the temperature at 200 DEG C 12h, is warming up to 850 DEG C later with the heating rate of 5 DEG C/min, and keep the temperature 3h,
Densification piezoelectric ceramics is made.
Embodiment 3
The preparation method of the potassium sodium niobate ceramic of the present embodiment, using following steps:
1) Nb is taken2O5, KOH, NaOH and deionized water be configured to suspension, wherein Nb2O5, KOH, NaOH three mole
Than for Nb2O5: KOH:NaOH=1:1:1, the concentration of KOH is 8mol/L in suspension；
2) K for being 50nm by suspension and partial size0.5Na0.5NbO3It is put into mold, hangs after powder ground and mixed 1.5min
The weight of supernatant liquid accounts for K0.5Na0.5NbO3The 33% of powder weight；
3) to the material uniaxial compression 435MPa in mold, it is incubated at room temperature pressure maintaining 10min, then with 10 DEG C/min's
Heating rate is warming up to 155 DEG C, and heat-insulation pressure keeping 100min obtains blank；
4) blank is kept the temperature at 200 DEG C 12h, is warming up to 900 DEG C later with the heating rate of 5 DEG C/min, and keep the temperature 4h,
Densification piezoelectric ceramics is made.
Embodiment 4
The preparation method of the potassium sodium niobate ceramic of the present embodiment, using following steps:
1) Nb is taken2O5, KOH, NaOH and deionized water be configured to suspension, wherein Nb2O5, KOH, NaOH three mole
Than for Nb2O5: KOH:NaOH=1:1:1, the concentration of KOH is 10mol/L in suspension；
2) K for being 65nm by suspension and partial size0.5Na0.5NbO3It is put into mold, suspends after powder ground and mixed 2min
The weight of liquid accounts for K0.5Na0.5NbO3The 40% of powder weight；
3) to the material uniaxial compression 432MPa in mold, it is incubated at room temperature pressure maintaining 15min, then with 10 DEG C/min's
Heating rate is warming up to 150 DEG C, and heat-insulation pressure keeping 120min obtains blank；
4) blank is kept the temperature at 200 DEG C 12h, is warming up to 700 DEG C later with the heating rate of 5 DEG C/min, and keep the temperature 3h,
Densification piezoelectric ceramics is made.
Embodiment 5
The preparation method of the potassium sodium niobate ceramic of the present embodiment, substantially the same manner as Example 1, difference is only that, KxNa1- xNbO3X=0.3 in powder, Nb2O5, KOH, NaOH three molar ratio be Nb2O5: KOH:NaOH=0.5:0.3:0.7.
Embodiment 6
The preparation method of the potassium sodium niobate ceramic of the present embodiment, substantially the same manner as Example 1, difference is only that, KxNa1- xNbO3X=0.7 in powder, Nb2O5, KOH, NaOH three molar ratio be Nb2O5: KOH:NaOH=0.5:0.7:0.3.
Comparative example
The preparation method of the potassium sodium niobate ceramic of comparative example, substantially the same manner as Example 1, difference is only that, suspension by
KOH, NaOH and deionized water are formulated, and the molar ratio of KOH, NaOH are KOH:NaOH=1:1, the concentration of KOH in suspension
For 5mol/L.
Experimental example
The performance of densification piezoelectric ceramics obtained by the preparation method embodiment 1-6 of this experimental example detection potassium sodium niobate ceramic refers to
Mark, the results are shown in Table 1.Wherein consistency test uses Archimedes's drainage, and piezoelectric constant measurement uses ZJ-3AN type d33
Tester detection, relative dielectric constant and dielectric loss use dielectric temperature spectral measurement system (impedance analyzer containing HP4294A), and
Curie temperature (T is determined according to temperature corresponding to relative dielectric constant maximum valueC)。
The performance indicator of the potassium sodium niobate ceramic of 1 embodiment and comparative example of table
| Consistency, % | Piezoelectric constant d33, pC/N | Curie temperature, DEG C | Relative dielectric constant | Dielectric loss | |
| Embodiment 1 | 92.7 | 110 | 412 | 695 | 0.03 |
| Embodiment 2 | 93.5 | 106 | 416 | 678 | 0.04 |
| Embodiment 3 | 95.6 | 136 | 424 | 726 | 0.02 |
| Embodiment 4 | 91.8 | 92 | 409 | 657 | 0.04 |
| Embodiment 5 | 93.1 | 85 | 402 | 641 | 0.04 |
| Embodiment 6 | 92.9 | 76 | 385 | 648 | 0.03 |
| Comparative example | 90.5 | 84 | 407 | 637 | 0.05 |
As shown in Table 1, the consistency of the potassium sodium niobate ceramic of embodiment reaches 91.8% or more, at room temperature, pressure
Electric constant d33Reach 76-136pC/N, Curie temperature reaches 385-424 DEG C, and relative dielectric constant reaches 641-726, dielectric loss
For 2-5%.Compared with comparative example, using the resulting K of the method for the present invention0.5Na0.5NbO3The consistency and piezoelectricity of ceramics sample
It can be improved largely.
Claims (7)
1. a kind of preparation method of potassium sodium niobate ceramic, which comprises the following steps: will be mainly by nanometer KxNa1- xNbO3Powder, niobium source, potassium resource, sodium source and solvent composition mixing abrasive lapping it is uniform after, temperature is 150-160 DEG C, pressure is
Block is pressed under 430-440MPa, be dried, be heat-treated later at 700 DEG C or more to get；
The niobium source, potassium resource, the dosage of sodium source meet KxNa1-xNbO3Stoichiometric ratio, after the heat treatment convert after be
KxNa1-xNbO3；KxNa1-xNbO3In, 0 < x < 1.
2. the preparation method of potassium sodium niobate ceramic as described in claim 1, which is characterized in that in mixture, the quality of solvent
Content is not more than 15%.
3. the preparation method of potassium sodium niobate ceramic as described in claim 1, which is characterized in that the time of compacting is 1-
120min。
4. the preparation method of potassium sodium niobate ceramic as claimed in claim 1 or 3, which is characterized in that temperature be 150-160
DEG C, pressure be 430-440MPa under suppress before, first room temperature, pressure be 430-440MPa under suppress 10-15min.
5. the preparation method of potassium sodium niobate ceramic as described in claim 1, which is characterized in that the time of heat treatment is 3-4h.
6. the preparation method of the potassium sodium niobate ceramic as described in any one of claim 1-3,5, which is characterized in that the mixing
Material is prepared by following steps: niobium source, potassium resource, sodium source and solvent being first configured to suspension, then by KxNa1-xNbO3Powder
Body and the suspension ground and mixed are uniform；The quality of suspension is nanometer KxNa1-xNbO3The 30-40% of powder quality.
7. the preparation method of potassium sodium niobate ceramic as claimed in claim 6, which is characterized in that the concentration of potassium resource is in suspension
2-10mol/L。
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Application publication date: 20190723 Assignee: Zhongshan Lvgao Building Materials Co.,Ltd. Assignor: HENAN University OF SCIENCE AND TECHNOLOGY Contract record no.: X2023980035142 Denomination of invention: A preparation method of potassium sodium niobate ceramics Granted publication date: 20211123 License type: Common License Record date: 20230428 |