CN113956039A - Preparation method of large-size high-quality potassium tantalate-niobate ceramic target - Google Patents
Preparation method of large-size high-quality potassium tantalate-niobate ceramic target Download PDFInfo
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Abstract
The invention belongs to the field of inorganic nonmetallic materials, relates to the preparation of artificial crystals and functional ceramic materials, and particularly relates to a preparation method of a large-size high-quality potassium tantalate-niobate ceramic target material. The preparation method comprises the following steps: cleaning potassium tantalate-niobate crystal waste to obtain a ceramic precursor, crushing and sieving the ceramic precursor to obtain precursor powder, mixing the precursor powder with a binder, granulating, and sequentially performing dry pressing, heating, binder removal and sintering on the granulated powder to obtain the powder; wherein, the process for cleaning the potassium tantalate niobate crystal waste comprises the following steps: and soaking the potassium tantalate-niobate crystal waste into an acid solution to remove alkaline components. The invention adopts the potassium tantalate niobate crystal waste as the raw material, realizes the reasonable reutilization of resources, and has no solid phase reaction in the manufacturing process, thereby having short sintering time, and the manufactured ceramic target material has uniform phase and controllable size.
Description
Technical Field
The invention belongs to the field of inorganic nonmetallic materials, relates to the preparation of artificial crystals and functional ceramic materials, and particularly relates to a preparation method of a large-size high-quality potassium tantalate-niobate ceramic target material.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Potassium tantalate niobate (KTa)1-xNbxO3(ii) a X is more than or equal to 0 and less than or equal to 1, abbreviated as KTN) ceramic sheet generally consists of K2CO3、Ta2O5、Nb2O5And sintering the metal oxide through solid-phase reaction. The inventor researches to find that potassium tantalate (KTaO) is caused by infinite solid solution characteristics of KTN crystal3KT) and potassium niobate (KNbO)3KN) have a large difference in internal crystal structure, resulting in a complicated internal structure of the material. The KTN crystal can exist in a paraelectric phase or a ferroelectric phase (a tetragonal phase or an orthorhombic phase) at room temperature according to different internal Ta/Nb ratios, and free ion transport cannot be realized due to solid phase reaction, so that Ta/Nb uniform distribution of the sintered and synthesized KTN ceramic is difficult to realize, and the phase of the KTN ceramic plate is complicated; at the same time, the solid phase should be CO2When the gas is released, pores are formed in the ceramic sheet, so that the ceramic sheet has poor compactness. In conclusion, due to non-uniform phases and poor compactness, the preparation of the KTN ceramic by the solid-phase reaction method is difficult to meet the application requirements of the KTN target.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a preparation method of a large-size high-quality potassium tantalate-niobate ceramic target material, which can provide a high-quality target source for a high-quality KTN film material.
In order to achieve the purpose, the technical scheme of the invention is as follows:
on the one hand, the application of the potassium tantalate niobate crystal waste material in preparing the potassium tantalate niobate ceramic target material is provided.
The KTN single crystal is another KTN target source for sputtering, is a solid solution mixed crystal of KT crystal and KN crystal, and is generally prepared by a melt method. However, the infinite solid solution property of the KTN crystal, the yield of the KTN single crystal is low, and the KTN single crystal which can not reach the optical, piezoelectric and dielectric application standards can only be used as a waste product and discarded; the available KTN single crystals have high requirements on crystal orientation, size and the like, so that the utilization rate of the KTN single crystals is low (the utilization rate of the KTN single crystals after being processed is less than 50 percent generally), and more leftovers are produced. The potassium tantalate niobate crystal waste is a KTN single crystal which cannot reach the optical, piezoelectric and dielectric application standards in the process of preparing the KTN single crystal by a melt method and a leftover which cannot be utilized after preparing the KTN single crystal.
According to the invention, the potassium tantalate niobate crystal waste is used as the raw material for preparing the potassium tantalate niobate ceramic target, so that the problem of poor compactness of the ceramic piece is solved by avoiding gas release caused by solid-phase reaction and preventing gas from generating pores inside the ceramic piece, and the sintering time is short and the cost is low.
Meanwhile, the potassium tantalate niobate crystal waste is used as a raw material, so that reasonable resource recycling is realized, and 'waste is changed into valuable'.
On the other hand, the preparation method of the large-size high-quality potassium tantalate-niobate ceramic target comprises the steps of cleaning potassium tantalate-niobate crystal waste to obtain a ceramic precursor, crushing and sieving the ceramic precursor to obtain precursor powder, mixing the precursor powder with a binder, granulating, and sequentially performing dry pressing, heating, binder removal and sintering on the granulated powder to obtain the large-size high-quality potassium tantalate-niobate ceramic target; wherein, the process for cleaning the potassium tantalate niobate crystal waste comprises the following steps: and soaking the potassium tantalate-niobate crystal waste into an acid solution to remove alkaline components.
In the preparation process of the KTN single crystal, defects or pits exist in crystal lattices, or gaps exist among formed crystals, so that raw materials are filled in the crystal lattices to form inclusions; meanwhile, in the growth process of the KTN single crystal, microcracks are generated under the action of stress, recrystallization is easy to generate in the microcracks, inclusions can be formed, the inclusions influence the growth of the KTN single crystal, and researches find that the defects of the inclusions influence the phase of the potassium tantalate niobate ceramic target material prepared by the inclusions, and meanwhile, the defects of the inclusions influence the uniform distribution of Ta/Nb, so that the formed phase of the KTN ceramic plate is relatively complex. Further research shows that the inclusion defects are mainly alkaline components, so that the inclusion defects can be removed through acid solution soaking, the uniformity of the prepared KTN ceramic phase can be ensured, and the increase of sintering time caused by the inclusion defects is eliminated.
In a third aspect, the potassium tantalate niobate ceramic target is obtained by the preparation method.
The potassium tantalate niobate ceramic target material obtained by the preparation method provided by the invention has the advantages of uniform phase, high density and large size, and can better meet the application requirements of KTN targets.
In a fourth aspect, the potassium tantalate niobate ceramic target is applied to preparing a KTN film material.
The invention has the beneficial effects that:
(1) the raw materials adopted by the embodiment of the invention are waste KTN crystal leftovers in the crystal processing process or grown KTN crystals with poor quality, so that the cost is saved, the environment is protected, and the invention has very bright popularization prospect.
(2) The large-size compact potassium tantalate niobate ceramic target provided by the embodiment of the invention has the advantages of short sintering time, uniform phase, high density, controllable size and wide application range.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is an X-ray diffraction spectrum of KTN ceramic target materials prepared in examples 1-3 of the present invention;
fig. 2 is a scanning electron microscope picture of the KTN ceramic sheet provided in embodiment 1 of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The potassium tantalate niobate crystal or single crystal is a KTa crystal with Nb component of 0-1, crystal phase of cubic (m3m), tetragonal (4mm) or orthorhombic (mm2) and doping ions of Cu, Fe, Sn, Ti, Li, Na and Mn which are singly doped or mixed and doped in multiple1-xNbxO3Or M: KTa1-xNbxO3And (4) crystals.
In view of the problems of non-uniform phase, poor density and the like of the existing potassium tantalate niobate ceramic target material, the invention provides a preparation method of a large-size high-quality potassium tantalate niobate ceramic target material.
The invention provides an application of potassium tantalate niobate crystal waste in preparation of a potassium tantalate niobate ceramic target material.
According to the invention, the potassium tantalate niobate crystal waste is used as the raw material for preparing the potassium tantalate niobate ceramic target, so that the problem of poor compactness of the ceramic piece is solved by avoiding gas release caused by solid-phase reaction and preventing gas from generating pores inside the ceramic piece, and the sintering time is short and the cost is low.
Meanwhile, the available KTN single crystal prepared at present has higher requirement, higher rejection rate and lower utilization rate, so the invention takes the potassium tantalate niobate crystal waste as the raw material and is easier to obtain.
The invention also provides a preparation method of the large-size high-quality potassium tantalate-niobate ceramic target material, which comprises the steps of cleaning potassium tantalate-niobate crystal waste to obtain a ceramic precursor, crushing and sieving the ceramic precursor to obtain precursor powder, mixing the precursor powder with a binder, granulating, and sequentially performing dry pressing, heating, binder removal and sintering on the granulated powder to obtain the large-size high-quality potassium tantalate-niobate ceramic target material; wherein, the process for cleaning the potassium tantalate niobate crystal waste comprises the following steps: and soaking the potassium tantalate-niobate crystal waste into an acid solution to remove alkaline components.
The invention can remove the inclusion defects by soaking in the acid solution, not only can ensure the uniformity of the phase of the prepared KTN ceramic, but also can eliminate the increase of sintering time caused by the inclusion defects.
In some examples of this embodiment, the acid solution is dilute hydrochloric acid. The dilute hydrochloric acid is hydrochloric acid with the mass fraction of less than 20%. Avoid corroding potassium tantalate niobate crystal.
In some examples of this embodiment, the process for cleaning potassium tantalate niobate crystal waste comprises: and soaking the potassium tantalate niobate crystal waste into acetone. The step is used for removing impurities such as 502 glue, paint and the like which are remained in the crystal processing process. The soaking time is preferably 2 to 3 hours.
In some examples of this embodiment, the process for cleaning potassium tantalate niobate crystal waste comprises: soaking the potassium tantalate niobate crystal waste into alcohol solution. This step is used to remove residual surface binders such as gums, waxes, etc. and organic impurities from the crystal processing, such as KTN crystal processing scraps. The soaking time is preferably 2 to 3 hours. The concentration of the alcohol solution is 95-99.5% (volume percentage).
In some examples of this embodiment, the process of washing the potassium tantalate niobate crystal waste comprises water washing. For removing impurity ions. Soaking in acid solution to remove alkaline components, and washing with water. The washing times are reduced, the flow is simplified, and the water is saved.
In some examples of this embodiment, the potassium tantalate niobate crystal waste is washed and then dried.
In order to ensure the improvement of material performance, the reduction of sintering temperature and the improvement of sintering quality, the crushing of raw materials aims to obtain high-purity and ultrafine powder as much as possible. Therefore, the invention needs to clean the waste potassium tantalate niobate crystal. In order to ensure the particle size of the powder, ball milling is generally adopted, however, impurities are inevitably introduced in the ball milling process, and the grinding time is not suitable to be too long in order to reduce impurity pollution caused by ball milling. Thus, in some examples of this embodiment, the time of the ball milling in the crushing and sieving is 22 to 26 hours. In the ball milling process, the mass ratio of the grinding balls to the ceramic precursor is 2: 0.9-1.1. In order to better avoid the introduction of impurities, the grinding balls are agate grinding balls. The rotation speed of the ball milling is preferably 100-150 r/min. The particle size of the precursor powder is preferably 200 to 300 mesh. When the particle size is too large, the crushing and sieving process may be repeated.
The ceramic target material preparation process requires that the granularity of the raw materials is as fine as possible, so that ball milling and crushing are required. However, the finer the powder, the poorer the fluidity, and the larger the specific surface area of the raw material and the larger the volume occupied, so that the powder cannot be uniformly filled in a steel mold during dry press molding, and it is difficult to perform the preform densely. The granulation process is usually adopted, i.e. the binder and the powder are fully mixed and sieved to form coarse powder particles with good flowability. The binder generally adopts organic compounds with binding characteristics, and the other remarkable effect of the organic compounds is to increase the plasticity of the blank and the strength of the blank. In some examples of this embodiment, the process of granulating is: heating the precursor powder and the binder until the binder is melted, mixing uniformly and sieving. The heating temperature should not be too high to prevent the adhesive from being damaged too much due to excessive temperature rise. The heating temperature is controlled to be well melted just when the binder is melted, and can be 1-10 ℃ higher than the melting temperature. And stirring after melting to uniformly mix the precursor powder and the binder. The purpose of sieving is to make the size of the particles similar so as to ensure the uniformity of the materials; after granulation is finished, the obtained powder has good flowability, is convenient to be pressed into compact and uniform wafers and cylinders by using a steel die, and the number of sieved meshes is 70-90 meshes. The binder can be paraffin, polyvinyl alcohol solution and the like. When the polyvinyl alcohol solution is used as the binder, the granulating process is carried out at room temperature because the polyvinyl alcohol solution is liquid.
And tabletting the granulated powder through a one-way pressurizing mould, wherein the pressure in the mould can generate obvious pressure gradient, and the pressure difference can also be generated in a blank body. Generally, the larger the molding pressure, the smaller the particle spacing, and the easier the sintering; however, if the forming pressure is too high, the plastic deformation limit of the material is exceeded, and the blank body is brittle and broken. In some examples of this embodiment, the dry-pressing pressure is 38 to 42 MPa. Dry pressing can be carried out using a round steel die with a diameter of 30 mm.
In the process of calcining the green body doped with the organic binder, the organic binder needs to undergo processes of melting, decomposition, volatilization and the like in the green body, so that the green body is deformed and cracked, and the mechanical strength is also reduced. Because the organic binder contains more carbon, when oxygen is insufficient to generate a reducing atmosphere, the sintering quality is influenced, the quality of a ceramic sample is reduced, and the final performance of a product is influenced. Therefore, the green body needs to be de-glued before calcination. Because the factors influencing the glue discharging process are many, the technological process of the glue discharging process needs to be comprehensively formulated according to the quantity and the type of the adhesive, the size and the shape of the blank, the properties of ingredients and the like in actual operation. In some examples of this embodiment, the temperature is programmed to 500-800 ℃ in an air atmosphere and maintained. The heating rate is 1-2 ℃/min. The heat preservation time is 2-3 h. For example, when the adhesive is paraffin, the heating rate is 1 ℃/min, the temperature is raised to 500 ℃, the temperature is kept at 500 ℃ for 2h, and the paraffin serving as the adhesive in the blank is discharged. When the binder is polyvinyl alcohol solution, the heating rate is 2 ℃/min, the temperature is raised to 750 ℃, the temperature is kept at 750 ℃ for 2h, and the polyvinyl alcohol serving as the binder in the blank body is discharged. When paraffin is used as the binder, the addition amount of the paraffin is 8-10% of the mass of the precursor powder. When the polyvinyl alcohol solution is used as a binder, the addition amount of the polyvinyl alcohol solution is 1-2 drops per gram of the precursor powder. The mass fraction of the polyvinyl alcohol solution is 6-8%.
The bond between the particles of the green body formed from the powder is mainly formed by mechanical engagement or binding with a plasticizer, and the green body is not strong. The blank is heated at a certain temperature, so that the mechanical occlusion between particles is changed into the direct bonding by ionic bonds and covalent bonds, the strength of the material is greatly improved, and the process is sintering. The sintering of the ceramic material is divided into three stages, namely a temperature rise stage, a heat preservation stage and a temperature reduction stage. In the temperature rising stage, the micro phenomena of volatile emission, decomposition and oxidation of organic adhesives and the like, liquid phase generation, grain rearrangement, growth and the like often appear in the green body. Operationally, different ramp rates are required at different stages in view of the removal of volatiles during sintering and the life of the sintering furnace. The holding phase refers to the process in which the parison is held at the maximum temperature to which it is raised, also commonly referred to as the sintering temperature. Powder sintering involves a solid-phase mass transfer process. Is a thermally activated process, the higher the temperature, the faster the sintering. The sintering temperature is related to the chemical characteristics of the crystal of the material, the crystal lattice energy is large, the mass point movement is difficult at high temperature, and the sintering is not facilitated. The cooling stage is the process from the highest temperature to the room temperature of the ceramic material, and the cooling process is accompanied by physicochemical changes such as liquid phase solidification, crystallization, phase change and the like. The cooling mode and the cooling speed have great influence on the composition, the structure, the performance and the like of the final phase of the ceramic material.
During sintering, if the temperature is too high, the green body may melt and deform, and if the sintering temperature is too low, the green body is not fully sintered, the bonding between material particles is not tight, and a large number of pores exist between crystal particles, which is not beneficial to further improving the compactness of the ceramic. In some examples of this embodiment, the temperature is programmed to 850-950 ℃ for a set time, then the temperature is continuously raised to 1150-1200 ℃ for a set time, and then the temperature is lowered. The heating rate for heating to 850-950 ℃ is preferably 4-6 ℃/min. The heat preservation time after the temperature is raised to 850-950 ℃ is preferably 0.5-1.5 h. The heating rate for heating to 1150-1200 ℃ is preferably 4-6 ℃/min. The heat preservation time after the temperature is raised to 1150-1200 ℃ is preferably 2-3 h. The cooling rate of the mixture to room temperature is 4-6 ℃/min.
In a third embodiment of the invention, a potassium tantalate niobate ceramic target is provided, which is obtained by the preparation method.
The potassium tantalate niobate ceramic target material obtained by the preparation method provided by the invention has the advantages of uniform phase, high density and large size, and can better meet the application requirements of KTN targets.
The fourth embodiment of the invention provides an application of the potassium tantalate niobate ceramic target material in preparation of KTN thin film materials.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
A preparation method of a potassium tantalate niobate ceramic target comprises the following steps:
1) cleaning and material preparation: taking a proper amount of waste leftovers discarded in the KTN crystal processing process, respectively soaking for 2h by using acetone solution, alcohol solution and dilute hydrochloric acid (the mass fraction is 10%) to remove 502 organic binders such as glue, gum, paraffin and the like and alkaline components, then washing for 3 times by using deionized water to remove acetone, alcohol and dilute hydrochloric acid remained on the surface of the material, and finally drying for 12h in a hot air oven.
2) Crushing and sieving: placing the clean and dry KTN crystal waste processed in the step 1) into a ball milling tank, wherein the ball-material ratio is 2:1, the rotating speed is 120r/min, and dry milling is carried out for 24 hours; and (3) sieving the ground raw material powder to obtain raw material powder with the particle size of 270-300 meshes, and repeating the step 2) on the residual material with larger particle size.
3) Wax frying and granulation: adding 10% of paraffin wax into the raw material powder obtained in the step 2), placing the raw material powder in a ceramic evaporation pan, slowly heating the raw material powder by using a universal electronic furnace, and continuously stirring the raw material powder by using a medicine spoon to uniformly mix the raw material powder. The heating temperature should not be too high to prevent the paraffin from being excessively heated and greatly lost. The temperature is controlled to just melt the paraffin. The end point of the wax frying is that the paraffin and the raw materials are uniformly mixed; after the wax frying is finished, sieving the mixture of the paraffin and the paraffin for granulation by a sieve of 80 meshes to obtain powder with uniform particle size;
4) dry pressing and forming: after granulation, an appropriate amount of mixture is weighed by using an electronic balance, and is subjected to cold press molding by using a steel die under the pressure of 40MPa to obtain a cylindrical ceramic blank with the diameter of 30mm, the thickness of 3mm, the diameter of 10mm and the height of 5 mm.
5) Heating and removing glue: placing the ceramic blank on a corundum plate, placing the corundum plate in a high-temperature sintering furnace, in the air atmosphere, heating at 0-500 ℃ at a heating rate of 1 ℃/min, keeping the temperature at 500 ℃ for 2h, and discharging paraffin serving as an adhesive;
6) sintering to form porcelain: after the temperature is raised and the cement is removed, the heating is continued. Heating to 900 ℃ at the heating rate of 5 ℃/min, keeping the temperature at 900 ℃ for 1h, then continuously heating to 1170 ℃ at the heating rate of 5 ℃/min, and keeping the temperature at 1170 ℃ for 2 h.
7) Cooling and sampling: and after the step 6) is finished, cooling at the cooling rate of 5 ℃/min until the temperature is room temperature. And taking out the sintered ceramic KTN ceramic target material at room temperature, wherein the XRD pattern of the obtained product is shown in figure 1, and the SEM scanning image is shown in figure 2.
The density of the ceramic target is characterized by the ratio of the actual density to the theoretical density of the ceramic target, and can be expressed by the formula (1):
the actual density of the ceramic target was determined by Archimedes drainage (Archimedes drainage) using an ohauss FR124CN analytical balance, in which process the formula (2) used was:
in the above formula, m1Represented is the dry weight (mass of sample in air), m2Represented by the float weight (mass of sample in water), m3Representative is the wet weight (weight of the sample after soaking for 24h and wiping off surface distilled water), ρ0Refers to the density of distilled water (at the time of measurement, the temperature was recorded and the density of distilled water was determined by referring to the instrument booklet).
The density of the KTN crystal is the theoretical density of the KTN ceramic target.
An XRD (X-ray diffraction) pattern shows that the finally obtained KTN ceramic target material has a uniform phase and the compactness reaches up to 93%.
Example 2
As in example 1 above, the difference is that:
the paraffin wax added in step 3) of example 1 was changed to a polyvinyl alcohol solution with a mass fraction of 7 wt%. Putting the raw material powder obtained in the step 2) into an agate mortar, dropwise adding a drop of polyvinyl alcohol solution into each gram of material, and grinding for 30min to uniformly mix the raw material powder and the polyvinyl alcohol binder. After grinding, sieving with a 80-mesh sieve for granulation.
The binder removal temperature in step 5) in example 1 was changed to 750 ℃, the temperature rise rate was 2 ℃/min, and the temperature was maintained at 750 ℃ for 2h to remove the polyvinyl alcohol as a binder from the green body.
Finally, the KTN ceramic target with uniform phase and 93.5% density is obtained. The XRD pattern of the obtained product is shown in figure 1.
Example 3
As in example 1 above, the difference is that:
the raw material selected in the step 1) in the example 1 is changed into KTN crystals which have poor growth, poor quality and can not meet the use requirement. Taking a proper amount of waste KTN crystals, and soaking the waste KTN crystals for 3 hours by using dilute hydrochloric acid to remove alkaline components in the waste crystals (mainly aiming at the KTN waste crystals with inclusion defects); then washing for 3 times by using deionized water to remove residual alcohol and other impurities remained on the surface of the waste crystal, and finally drying in a hot air oven for 12 hours;
finally, the KTN ceramic target with uniform phase and 93.8% density is obtained. The XRD pattern of the obtained product is shown in figure 1.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An application of potassium tantalate niobate crystal waste in preparing potassium tantalate niobate ceramic target raw materials.
2. A preparation method of a large-size high-quality potassium tantalate-niobate ceramic target is characterized in that potassium tantalate-niobate crystal waste is cleaned to obtain a ceramic precursor, the ceramic precursor is crushed and sieved to obtain precursor powder, the precursor powder is mixed with a binder and then granulated, and the granulated powder is subjected to dry pressing, heating, binder removal and sintering in sequence to obtain the target; wherein, the process for cleaning the potassium tantalate niobate crystal waste comprises the following steps: and soaking the potassium tantalate-niobate crystal waste into an acid solution to remove alkaline components.
3. The method for preparing a large-size high-quality potassium tantalate-niobate ceramic target according to claim 2, wherein the acid solution is dilute hydrochloric acid;
or the process for cleaning the potassium tantalate niobate crystal waste comprises the following steps: soaking the potassium tantalate niobate crystal waste into acetone;
or the process for cleaning the potassium tantalate niobate crystal waste comprises the following steps: soaking the potassium tantalate niobate crystal waste into an alcohol solution;
or the process of cleaning the potassium tantalate niobate crystal waste comprises water washing;
or, cleaning the potassium tantalate niobate crystal waste and then drying.
4. The method for preparing the large-size high-quality potassium tantalate-niobate ceramic target according to claim 2, wherein the ball milling time is 22-26 hours in crushing and sieving; preferably, in the ball milling process, the mass ratio of the milling balls to the ceramic precursor is 2: 0.9-1.1; preferably, the grinding balls are agate grinding balls; preferably, the rotation speed of the ball milling is preferably 100-150 r/min; preferably, the particle size of the precursor powder is 200 to 300 mesh.
5. The method for preparing the large-size high-quality potassium tantalate-niobate ceramic target material as claimed in claim 2, wherein the granulation process comprises: heating the precursor powder and the binder until the binder is melted, mixing uniformly and sieving.
6. The method for preparing a large-size high-quality potassium tantalate-niobate ceramic target according to claim 2, wherein the dry-pressing pressure is 38 to 42 MPa.
7. The method for preparing a large-size high-quality potassium tantalate-niobate ceramic target according to claim 2, wherein the temperature is programmed to 500-800 ℃ in an air atmosphere and the temperature is maintained.
8. The method for preparing a large-size high-quality potassium tantalate-niobate ceramic target according to claim 2, wherein the temperature is programmed to 850-950 ℃, the temperature is maintained for a set time, then the temperature is continuously raised to 1150-1200 ℃, and the temperature is reduced after the temperature is maintained for the set time.
9. A potassium tantalate niobate ceramic target material, which is characterized by being obtained by the preparation method of any one of claims 2 to 8.
10. The use of the potassium tantalate niobate ceramic target of claim 9 as a target for the preparation of KTN thin film materials.
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| CN116396076B (en) * | 2023-04-04 | 2024-04-26 | 基迈克材料科技（苏州）有限公司 | Preparation method of conductive lithium niobate target material |
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