CN109208066B - Single crystal preparation method of ferroelectric ceramic compound - Google Patents
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Abstract
The invention relates to a single crystal preparation method of a ferroelectric ceramic compound. The preparation method comprises the following steps: preparing a ferroelectric ceramic block by solid-phase reaction, and further ball-milling the ferroelectric ceramic block into micron powder of more than 200-2000 meshes; preparing ferroelectric ceramic precursor sol by a sol-gel method, and further drying to obtain amorphous ferroelectric ceramic dry gel powder; and wet-grinding the micron powder and the dry gel powder into slurry in a solvent, preparing a biscuit sample and sintering in a sintering furnace. Compared with the prior art, the invention has the following advantages: under the condition of no participation of a liquid phase and low sintering temperature, the ferroelectric ceramic single crystal with high quality and high purity and all fixed components with the molar ratio of 0-100 can be prepared; simple process, low cost, strong reproducibility, no need of complex preparation process and harsh single crystal growth conditions.
Description
Technical Field
The invention belongs to the technical field of single crystal preparation, and particularly relates to a single crystal preparation method of ferroelectric ceramic compounds.
Background
Ferroelectric ceramics (ferroelectric ceramics) material refers to a class of materials that have a ferroelectric effect. The main properties of ferroelectric ceramics are:
(1) the ferroelectric material is characterized by what is also called "ferroelectric phenomenon" or "ferroelectric effect": the crystal structure of the material has spontaneous polarization phenomenon under the condition of no external electric field, and the direction of the spontaneous polarization can be reversed or reoriented by the external electric field.
(2) When the ferroelectric material is subjected to phase transition, the dielectric constant peaks and Curie temperature (T) existsc) (ii) a When the temperature is higher than TcWhen the spontaneous polarization disappears, the ferroelectric phase is changed into the paraelectric phase, and the dielectric property follows Curie-Weiss law.
(3) The ferroelectric material has many properties such as piezoelectric property, dielectric property, pyroelectric property, photoelectric effect, acousto-optic effect, photorefractive effect and nonlinear optical effect besides ferroelectric property.
The characteristics of the ferroelectric ceramic determine its use. The ferroelectric memory can be used for manufacturing capacitors with large capacity, high-frequency micro capacitors, high-voltage capacitors, laminated capacitors, semiconductor ceramic capacitors and the like by utilizing the high dielectric constant, and can be used for manufacturing a ferroelectric memory with high storage capacity by utilizing a hysteresis loop formed by the change of the polarization direction along with the change of an external electric field; the dielectric amplifier, the waveguide tube and the phase shifter can be manufactured by utilizing the electro-optic effect that the dielectric constant of the electro-optic device changes in a nonlinear way along with an external electric field; the photoelectric effect of the material can be used for preparing optical memories, light valves, light modulators and the like; by utilizing the pyroelectric property, an infrared detector and the like can be manufactured. Various piezoelectric devices, actuators, sensors, and the like can be manufactured by utilizing the piezoelectricity. At present, ferroelectric materials are mainly developed for high energy storage density and electrocaloric effect in novel energy research. The electrocaloric effect of ferroelectric materials is one of the most competitive and promising materials for preparing new generation solid state refrigerator to replace Freon which is a liquid state refrigerator with environment destruction.
Currently, worldwide ferroelectric components are being produced in billions of dollars per year. Ferroelectric materials are a relatively large family, the best currently used being the ceramic family, which has been widely used in military and industrial applications.
A relatively common ferroelectric ceramic has Pb (Zr, Ti) O3(PZT) based, PbTiO3(PT) -series, PbZrO3(PZ) -based, (Pb, Ba) (Zr, Ti) O3Series, Pb (Zr, Sn, Ti) O3(PZST) -based Pb (Mg, Nb) O3(PMN) type, (Ba, Sr) TiO3(BST) -based, BaTiO3(BT) based, (Ba, Zr) TiO3(BZT)、KNbO3(KN) and K (Nb, Na) O3ABO of (KNN) series3A perovskite structure.
Ceramics can be divided into two broad categories, polycrystalline and single crystal. Because the single crystal ceramic is not influenced by grain size, grain orientation, grain boundaries, porosity and the like, the single crystal ceramic has more excellent performance than polycrystalline ceramics, such as more excellent dielectric, ferroelectric and optical properties and the like.
The main methods for preparing single crystals of ferroelectric ceramics are: optical float zone method, cosolvent method, Czochralski method, laser heating method, Bridgman method, etc. The method has the advantages of high purity requirement of raw materials, expensive equipment, complex process, difficult process control, higher crystallization temperature requirement and difficult obtainment of high-quality single crystals with fixed components.
Disclosure of Invention
The invention provides a single crystal preparation method of a ferroelectric ceramic compound, which is used for solving the problem of difficulty in single crystal preparation at present.
In order to solve the technical problems, the technical scheme of the invention is as follows: the single crystal preparation method of the ferroelectric ceramic compound comprises the following steps:
1) preparing a ferroelectric ceramic block with a set component through a solid-phase reaction, and further ball-milling the ferroelectric ceramic block into micron powder with the particle size of more than 200-2000 meshes;
2) preparing ferroelectric ceramic precursor sol by a sol-gel method, and further drying to obtain amorphous ferroelectric ceramic dry gel powder with set components;
3) wet-grinding the micron powder in the step 1) and the dry gel powder in the step 2) into slurry in a solvent, drying the slurry, pressing the dried slurry into a biscuit sample, sintering the biscuit sample in a sintering furnace, and cooling the biscuit sample to room temperature along with the furnace after sintering to obtain the ferroelectric ceramic single crystal product with set components.
Optionally, the ferroelectric ceramic is ABO3Perovskite structure, preferably PZT and BST series ferroelectric ceramics.
The ABO3The perovskite structure ferroelectric ceramic is commonly Pb (Zr, Ti) O3(PZT) based, PbTiO3(PT) -series, PbZrO3(PZ) -based, (Pb, Ba) (Zr, Ti) O3Series, Pb (Zr, Sn, Ti) O3(PZST) -based Pb (Mg, Nb) O3(PMN) type, (Ba, Sr) TiO3(BST) -based, BaTiO3(BT) based, (Ba, Zr) TiO3(BZT)、KNbO3(KN) or K (Nb, Na) O3(KNN) -based compound.
Optionally, the solid-phase reaction process in the step 1) is to calcine the mixture in a muffle furnace after ball milling and mixing, wherein the calcining temperature is the temperature obtained by subtracting 100-300 ℃ from the sintering temperature of the ferroelectric ceramic compound, and the temperature is kept for 2-7 hours.
Optionally, in the step 1), the process of preparing the block into the micron powder specifically includes firstly smashing the block in a mortar, sieving with a 40-200 mesh sieve, then ball-milling for 24 hours with an alcohol solvent as a medium, drying, and sieving with a 200-2000 mesh sieve.
Optionally, the complexing agent in the sol-gel method is a polymer material, preferably, polyvinylpyrrolidone (PVP) or citric acid.
Optionally, the solubility of the ferroelectric ceramic precursor sol in the step 2) is 0.1-1.0 mol/L.
Optionally, in the sol-gel method, deionized water, isopropanol, acetic acid, absolute ethyl alcohol or/and ethylene glycol methyl ether are/is used as
Optionally, in the step 3), the mass ratio of the micron powder to the dry gel powder is (3-20): 100.
Optionally, in the step 3), the preparation process of the slurry is specifically that the micron powder and the dry gel powder are wet-milled by taking an alcohol solvent as a medium to form a slurry, and the slurry is taken out and dried in a drying oven at the drying temperature of 100-300 ℃; and pressing the dried slurry powder into a biscuit sample under the pressure of 1-10 MPa, placing the biscuit sample into a sintering furnace for sintering, and preserving heat for 2-10 hours to finish sintering.
Optionally, the alcoholic solvent is methanol, ethanol or isopropanol.
Optionally, in step 3), the sintering temperature in the sintering furnace is below 1350 ℃.
Compared with the prior art, the technical scheme provided by the invention has the following advantages:
1) high quality high purity single crystals: the invention provides a method for preparing micron seed crystal by adopting a conventional solid phase reaction method, which is used for preparing high-quality single crystal by inducing mesoscopic crystal grains with the same components prepared by sol-gel as a crystal source, and no liquid phase participates in the crystal growth process. The ferroelectric ceramic single crystal with high quality and high purity and all fixed components with the molar ratio of 0-100 can be prepared.
2) The sintering temperature is low: calcined micron powder is used as seed crystal, amorphous dry gel powder is used as crystal source for seed crystal growth, and the single crystal with different crystal orientations can be prepared at the sintering temperature not higher than 1350 ℃ just like cloning seed crystal.
3) The method provided by the invention has the advantages of simple process, low cost, repeatable process and no need of complex preparation process and harsh single crystal growth conditions; expensive and high-energy consumption equipment is not needed, and the preparation of the ferroelectric single crystal with high quality and high purity is extremely easy to realize.
Drawings
FIG. 1 is Ba prepared in example 10.60Sr0.40TiO3XRD pattern of sintered body ceramic;
FIGS. 2a, 2b are Ba prepared in example 10.60Sr0.40TiO3SEM photograph of sintered body ceramic natural surface magnified 100 times;
FIG. 3a is Ba prepared in example 10.60Sr0.40TiO3TEM-SAED images of large-grain slices of sintered body ceramics, wherein the insert in the upper right corner is a 3D image of the large-grain slice in FIG. 2 b;
FIG. 3b is Ba prepared in example 10.60Sr0.40TiO3HRTEM of large grain slices of sintered body ceramics.
Detailed Description
For the sake of understanding, the following description will be made of a method for preparing a single crystal of a ferroelectric ceramic-based compound with reference to examples, which are intended to illustrate the present invention and not to limit the scope of the present invention.
In this example, the reagents and raw materials are commercially available, unless otherwise specified, and PVP used herein is PVP-K30 having a K value in the range of about 30.
Example 1: BST with barium-strontium ratio of 60:40 (mol%)
1) Solid-phase reaction: with BaTiO3、SrTiO3Is taken as a raw material and is represented by the chemical formula: ba0.60Sr0.40TiO3Mixing, wet grinding with anhydrous ethanol as medium for 2 hr, oven drying, and pressing to obtain blocks with diameter of 15 × 15mm2Putting the mixture into a muffle furnace, and keeping the temperature of 1175 ℃ for 7 hours for calcination; crushing the calcined block, sieving with a 40-mesh sieve, ball-milling for 24 hours, drying, sieving with a 200-mesh sieve, and preparing micron-sized calcined Ba at 1175 DEG C0.60Sr0.40TiO3Powder;
2) sol-gel process: dissolving PVP in isopropanol at room temperature, and dripping titanic acidAdding butyl ester into the solution of PVP-isopropanol, and stirring for 2 hours at normal temperature by using a magnetic stirrer to prepare a solution of tetrabutyl titanate-PVP-isopropanol; adding barium acetate and strontium acetate with a molar ratio of 60:40 into glacial acetic acid, stirring and heating to 110 ℃ by using a magnetic stirrer, keeping the temperature for 10 minutes until the barium acetate and the strontium acetate are completely dissolved, cooling to 80 ℃, slowly dropwise adding the solution into the tetra-n-butyl titanate-PVP-isopropanol solution, and stirring for 15-30 minutes after dropwise adding is finished to obtain barium strontium titanate precursor sol with the concentration of 0.4 mol/L; drying the precursor sol in a drying oven at 120 deg.C for 24 hr to obtain amorphous (Ba)0.60Sr0.40TiO3) Dry gel powder;
3) growing a single crystal: micron grade Ba in step 1)0.60Sr0.40TiO3The powder is used as a doping raw material, namely seed crystal, and the amorphous Ba in the step 2)0.60Sr0.40TiO3The dry gel powder is used as a main raw material as a crystal source, and the mass ratio of the micron powder to the dry gel powder is 10: 100; wet grinding the mixed powder for 2 hours by using isopropanol as a ball milling medium, taking out and drying the mixed powder, and pressing the mixed powder under the pressure of 2MPa to form phi 10 x 10mm without granulation2Biscuit samples; and horizontally placing the biscuit sample in a muffle furnace, directly heating the biscuit sample, and keeping the temperature at 1350 ℃ for 7 hours to obtain the sintered body ceramic.
As shown in fig. 1-2, microstructural analysis showed that the ceramic had distinct large grains of 100 to 300 μm in size, with intact crystal forms and a clear structure. As shown in fig. 3, which is a dot-matrix diagram rather than a concentric circular diagram, it can be shown that a single crystal of barium strontium titanate with a single barium strontium ratio is obtained, in which the lattice constant is identified, the crystal is a cubic system, the space group is Pm-3m (221), and the unit cell parameters are: α - β - γ -90 °,
the unit cell volume is:
example 2: BST with 75:25 (mol%) barium-strontium ratio
See example 1 for the preparation, except that in step 1 according to the formula: ba0.75Sr0.25TiO3Batching is carried out, and the molar ratio of the barium acetate to the strontium acetate in the step 2) is 75: 25.
Example 3: PZT with zirconium-titanium ratio of 53:47 mol%
1) Solid-phase reaction: with Pb3O4、ZrO2And TiO2Is taken as a raw material and is represented by the chemical formula: pb (Zr)0.53Ti0.47)O3Mixing, wet grinding with anhydrous ethanol as medium for 2 hr, oven drying, and pressing to obtain blocks with diameter of 15 × 15mm2Putting the mixture into a muffle furnace, and keeping the temperature at 1000 ℃ for 7 hours for calcination; crushing the calcined block, sieving with a 40-mesh sieve, ball-milling for 24 hours, drying, sieving with a 200-mesh sieve, and preparing micron-sized Pb (Zr) calcined at 1000 ℃0.53Ti0.47)O3Powder;
2) sol-gel process: completely dissolving PVP in isopropanol at room temperature, dropwise adding tetrabutyl titanate into a PVP-isopropanol solution, then adding tetrabutyl zirconate, wherein the molar ratio of tetrabutyl zirconate to tetrabutyl titanate is 53:47, and stirring for 2 hours at room temperature by using a magnetic stirrer to prepare a tetrabutyl titanate-tetrabutyl zirconate-PVP-isopropanol solution; adding lead acetate into ethylene glycol monomethyl ether, stirring and heating to 120 ℃ by using a magnetic stirrer, keeping the temperature for 30 minutes until the lead acetate is completely dissolved, cooling to 80 ℃, slowly dropwise adding a solution of tetrabutyl titanate-tetrabutyl zirconate-PVP-isopropanol into the lead acetate-ethylene glycol monomethyl ether solution, and stirring for 15-30 minutes after dropwise adding is finished to obtain lead zirconate titanate precursor sol with the concentration of 0.4 mol/L; drying the precursor sol in a drying oven at 120 deg.C for 24 hr to obtain amorphous Pb (Zr)0.53Ti0.47)O3) Dry gel powder;
3) growing a single crystal: micron-sized Pb (Zr) in step 1)0.53Ti0.47)O3The powder is used as a doping raw material, namely seed crystal, and amorphous Pb (Zr) in the step 2)0.53Ti0.47)O3The dry gel powder is taken as a main raw material and is used as a crystal source, and the mass ratio of the micron powder to the dry gel powder is 10: 100; using isopropanol as ball milling medium, adding the mixed powderWet grinding for 2 hr, taking out, drying, and press molding under 2MPa to obtain product with diameter of 10 × 10mm2Biscuit samples; and horizontally placing the biscuit sample in a muffle furnace, directly heating the biscuit sample, and keeping the temperature at 1200 ℃ for 7 hours to obtain the sintered body ceramic. Microstructure analysis shows that the ceramic has obvious large-grain single crystal with the size of more than 1mm, complete crystal form and clear structure.
Example 4 zirconium titanium ratio 10:90 mol%
See example 1 for the preparation, with the difference that in step 1) according to the formula: pb (Zr)0.10Ti0.90)O3Batching is carried out, and the molar ratio of the tetrabutyl zirconate to the tetrabutyl titanate in the step 2) is 10: 90.
Example 5
The difference from the embodiment 3 is that firstly, in the step 1), micron powder is sieved by a 1000-mesh sieve; secondly, in the step 2), the solubility of the lead zirconate titanate precursor sol is 0.1 mol/L; thirdly, in the step 3), the sintering temperature is 650 ℃, and the grain diameter of the sintered single crystal is 0.5-1 μm.
Finally, it should be noted that: the above examples are only for illustrating the technical solutions of the present invention, and are not limited thereto. Although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: it is to be understood that modifications may be made to the technical solutions described in the foregoing embodiments, or some or all of the technical features may be equivalently replaced, and such modifications or replacements may not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (6)
1. A single crystal preparation method of a ferroelectric ceramic compound is characterized by comprising the following steps:
step 1): preparing a ferroelectric ceramic block with a set component through a solid-phase reaction, wherein the solid-phase reaction process comprises the steps of calcining in a muffle furnace after ball milling and mixing, keeping the temperature for 2-7 hours at a temperature which is less than 100-300 ℃ of the sintering temperature of a corresponding ferroelectric ceramic compound, and further ball milling into 200-2000-mesh micron powder, wherein the ferroelectric ceramic is PZT and BST series ferroelectric ceramic;
step 2): preparing ferroelectric ceramic precursor sol by adopting a sol-gel method, adding a complexing agent into the sol-gel method, and further drying to obtain amorphous ferroelectric ceramic dry gel powder with set components;
step 3): wet grinding the micron powder in the step 1) and the dry gel powder in the step 2) into slurry in a solvent, wherein the mass ratio of the micron powder to the dry gel powder is (3-20): 100, drying the slurry, pressing the dried slurry into a biscuit sample under the pressure of 1-10 MPa, sintering the biscuit sample in a sintering furnace at the sintering temperature of below 1350 ℃, preserving the heat for 2-10 hours to complete sintering, and cooling the sintered biscuit sample to room temperature along with the furnace to obtain a ferroelectric ceramic single crystal product with set components.
2. The method for preparing a single crystal of a ferroelectric ceramic compound according to claim 1, wherein in step 1), the block is made into a micron powder by crushing the block in a mortar, sieving with a 40-200 mesh sieve, ball-milling with an alcohol solvent as a medium for 24 hours, drying, and sieving with a 200-2000 mesh sieve.
3. A single crystal preparation method of a ferroelectric ceramic like compound as in claim 1, wherein the complexing agent in the sol-gel method is polyvinylpyrrolidone or citric acid.
4. The method for preparing a single crystal of a ferroelectric ceramic compound according to claim 1, wherein the solubility of the ferroelectric ceramic precursor sol of step 2) is 0.1 to 1.0 mol/L.
5. A method for preparing a single crystal of a ferroelectric ceramic compound as in claim 1, wherein deionized water, isopropyl alcohol, acetic acid, absolute ethyl alcohol or/and ethylene glycol methyl ether are/is used as a solvent in the sol-gel method.
6. The method for preparing a single crystal of a ferroelectric ceramic compound as in claim 1, wherein in the step 3), the process for preparing the slurry is to wet-grind the micro powder and the dry gel powder by using an alcohol solvent as a medium to form the slurry, take out the slurry and dry the slurry in a drying oven at a temperature of 100-300 ℃.
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