CN107176837B - Preparation method of potassium tantalate niobate ceramic with ultrahigh dielectric constant - Google Patents
Preparation method of potassium tantalate niobate ceramic with ultrahigh dielectric constant Download PDFInfo
- Publication number
- CN107176837B CN107176837B CN201710400616.1A CN201710400616A CN107176837B CN 107176837 B CN107176837 B CN 107176837B CN 201710400616 A CN201710400616 A CN 201710400616A CN 107176837 B CN107176837 B CN 107176837B
- Authority
- CN
- China
- Prior art keywords
- potassium tantalate
- dielectric constant
- niobate
- ceramic
- aqueous solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
- C04B35/6266—Humidity controlled drying
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62675—Thermal treatment of powders or mixtures thereof other than sintering characterised by the treatment temperature
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A method for preparing potassium tantalate niobate ceramic with ultrahigh dielectric constant. The invention relates to the field of preparation of functional ceramic materials, in particular to a preparation method of potassium tantalate niobate ceramic with a high dielectric constant. The invention aims to solve the problem that the application of the existing potassium tantalate-niobate ceramic in the field of dielectric materials is limited due to low dielectric constant of the existing potassium tantalate-niobate ceramic. The method comprises the following steps: firstly, preparing rod-shaped potassium tantalate-niobate powder; secondly, preparing the potassium tantalate niobate ceramic with the ultrahigh dielectric constant. The method is used for preparing the potassium tantalate niobate ceramic with the ultrahigh dielectric constant.
Description
Technical Field
The invention relates to the field of preparation of functional ceramic materials, in particular to a preparation method of potassium tantalate niobate ceramic with a high dielectric constant.
Background
The rapid development of electronic information technology, miniaturization, integration and high capacity of electronic devices are important factors for promoting the development of the microelectronic industry, so that high dielectric constant materials have more and more important positions in the microelectronic field. The higher the dielectric constant of the material, the greater the specific capacitance of the capacitor when the device is shaped. Ferroelectric ceramics have a high dielectric constant and are one of the important electronic ceramic materials for manufacturing ferroelectric ceramic capacitors in the electronics industry. However, the traditional lead-based ceramic material contains a large amount of lead element, so that the traditional lead-based ceramic material has serious harm to the environment and the health of human beings. With the increasing awareness of environmental protection, the research on lead-free ceramic materials is receiving more and more attention. The potassium tantalate niobate (KTa1-xNbxO3, KTN) ceramic is a lead-free functional ceramic material with excellent performance. Different from other ferroelectric ceramics, the phase structure and the performance of the potassium tantalate niobate ceramic can be adjusted by adjusting the ratio of tantalum to niobium.
Through a literature search of the prior art, Jojoba et al have prepared potassium sodium niobate-based ceramics { (1-x) (K0.5Na0.5) NbO3-xSrTiO3, KNN-STO }, and have found that the relative dielectric constant of the KNN-STO ceramic is the greatest when x is 0.15. At a frequency of 100Hz, about 2000 is achieved. SrTiO3-PbTiO3-Bi2O 3.3 TiO2 series dielectric materials are modified by the Huangjiawei et al by compositely adding MgTiO3, CaTiO3, MnO2, Nb2O5 and SiO2 to prepare the ceramic capacitor material with the relative dielectric constant of 1500-2000.
chinese patent with publication number CN102515739A discloses a preparation method of high-dielectric ceramic, wherein the main phase of the high-dielectric ceramic is Ca2CuO3, and the dielectric constant of the high-dielectric ceramic is 3000-4000 at the frequency of 104-105 Hz.
Disclosure of Invention
The invention provides a preparation method of potassium tantalate niobate ceramic with ultrahigh dielectric constant, aiming at solving the problem that the application of the existing potassium tantalate niobate ceramic in the field of dielectric materials is limited due to low dielectric constant.
The preparation method of the potassium tantalate niobate ceramic with the ultrahigh dielectric constant is specifically carried out according to the following steps:
Firstly, preparing rod-shaped potassium tantalate-niobate powder: adding tantalum pentoxide and niobium pentoxide into a potassium hydroxide aqueous solution, magnetically stirring for 20-40 min, transferring to a hydrothermal reaction kettle, reacting for 20-30 h at 160-190 ℃, naturally cooling to room temperature after the reaction is finished, washing the product to be neutral by distilled water, putting the product into a vacuum drying oven, vacuumizing to 0.01MPa, and heating for 20-30 h at 60-85 ℃ to obtain rod-shaped potassium tantalate-niobate nano powder; the molar ratio of the tantalum pentoxide to the niobium pentoxide is 1: 1; the concentration of the potassium hydroxide aqueous solution is 8-9 mol/L; the molar ratio of the niobium pentoxide to the potassium hydroxide aqueous solution is 1 (60-70);
Secondly, uniformly mixing the rodlike potassium tantalate-niobate nano powder with a polyvinyl alcohol aqueous solution to obtain a mixture; pressing the mixture under 10Mpa to obtain cylindrical sheet with diameter of 12 mm; putting the pressed cylindrical sheet into a muffle furnace, removing glue for 4h at the temperature of 550 ℃, and then sintering for 2h at the temperature of 1075-1125 ℃ to obtain the potassium tantalate-niobate ceramic with the ultrahigh dielectric constant; the mass fraction of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 5-10%; the mass ratio of the polyvinyl alcohol aqueous solution to the rodlike potassium tantalate niobate nano powder is (1-10): 100.
The invention has the beneficial effects that: the method prepares the rod-shaped potassium tantalate-niobate nano powder by controlling the preparation process of the hydrothermal method, and the prepared rod-shaped potassium tantalate-niobate nano powder has larger polarization in unit volume, so that the material can obtain larger dielectric constant. Meanwhile, the interfacial polarization of the ceramic is related to the interfacial area among crystal grains in the ceramic, and the BET specific surface area (30.96m2/g) of the rodlike potassium tantalate-niobate nano powder is far larger than that (7.36m2/g) of the common potassium tantalate-niobate nano powder through the BET specific surface area test of the rodlike potassium tantalate-niobate nano powder and the common potassium tantalate-niobate nano powder. The invention takes the rodlike potassium tantalate niobate nano powder as the raw material to prepare the potassium tantalate niobate ceramic with the ultrahigh dielectric constant. The novel method for preparing the potassium tantalate niobate ceramic with the ultrahigh dielectric constant greatly widens the application of the potassium tantalate niobate ceramic in the field of dielectric materials, and can be applied to energy storage capacitors. At a frequency of 100Hz, the relative dielectric constant of the rod-shaped potassium tantalate-niobate ceramic is as high as 1.97X 104, while the relative dielectric constant of the common potassium tantalate-niobate ceramic is only 2.52X 103. The relative dielectric constant (2.81X 103) of the rod-shaped potassium tantalate-niobate ceramic is much higher than that (1.52X 103) of the common potassium tantalate-niobate ceramic even at a frequency of 106 Hz.
Drawings
FIG. 1 is an X-ray diffraction pattern of the rod-shaped potassium tantalate-niobate nano powder obtained in the first step of the example;
FIG. 2 is an X-ray diffraction diagram of a common potassium tantalate niobate nano-powder;
FIG. 3 is a scanning electron microscope image of the rod-shaped potassium tantalate-niobate nano powder obtained in the first step of the example;
FIG. 4 is a scanning electron microscope image of a common potassium tantalate niobate nano powder;
FIG. 5 is a graph showing the dielectric spectrum of the ultra-high dielectric constant potassium tantalate-niobate ceramic obtained in step two of example;
FIG. 6 is a graph of the dielectric spectrum of potassium tantalate niobate ceramic.
Detailed Description
The first embodiment is as follows: the preparation method of the potassium tantalate niobate ceramic with the ultrahigh dielectric constant is specifically carried out according to the following steps:
firstly, preparing rod-shaped potassium tantalate-niobate powder: adding tantalum pentoxide and niobium pentoxide into a potassium hydroxide aqueous solution, magnetically stirring for 20-40 min, transferring to a hydrothermal reaction kettle, reacting for 20-30 h at 160-190 ℃, naturally cooling to room temperature after the reaction is finished, washing the product to be neutral by distilled water, putting the product into a vacuum drying oven, vacuumizing to 0.01MPa, and heating for 20-30 h at 60-85 ℃ to obtain rod-shaped potassium tantalate-niobate nano powder; the molar ratio of the tantalum pentoxide to the niobium pentoxide is 1: 1; the concentration of the potassium hydroxide aqueous solution is 8-9 mol/L; the molar ratio of the niobium pentoxide to the potassium hydroxide aqueous solution is 1 (60-70);
Secondly, uniformly mixing the rodlike potassium tantalate-niobate nano powder with a polyvinyl alcohol aqueous solution to obtain a mixture; pressing the mixture under 10Mpa to obtain cylindrical sheet with diameter of 12 mm; putting the pressed cylindrical sheet into a muffle furnace, removing glue for 4h at the temperature of 550 ℃, and then sintering for 2h at the temperature of 1075-1125 ℃ to obtain the potassium tantalate-niobate ceramic with the ultrahigh dielectric constant; the mass fraction of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 5-10%; the mass ratio of the polyvinyl alcohol aqueous solution to the rodlike potassium tantalate niobate nano powder is (1-10): 100.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: and in the first step, the mixture is magnetically stirred for 20-40 min and then transferred to a hydrothermal reaction kettle. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: in the first step, the reaction is carried out for 24 hours at the temperature of 180 ℃. The other is the same as in the first or second embodiment.
the fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: and in the second step, the mass fraction of the polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 8%. The others are the same as in one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the concentration of the potassium hydroxide aqueous solution in the first step is 8.5 mol/L. The other is the same as one of the first to fourth embodiments.
the sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the molar ratio of the niobium pentoxide to the potassium hydroxide aqueous solution in the first step is 1: 68. The other is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and in the second step, the mass fraction of the polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 8%. The other is the same as one of the first to sixth embodiments.
the specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: and the mass ratio of the polyvinyl alcohol aqueous solution to the rodlike potassium tantalate-niobate nano powder in the second step is 3: 100. The other is the same as one of the first to seventh embodiments.
the beneficial effects of the present invention are demonstrated by the following examples:
Example (b): the preparation method of the potassium tantalate niobate ceramic with the ultrahigh dielectric constant specifically comprises the following steps:
Firstly, preparing rod-shaped potassium tantalate-niobate powder: adding tantalum pentoxide and niobium pentoxide into a potassium hydroxide aqueous solution, magnetically stirring for 30min, transferring to a hydrothermal reaction kettle, reacting for 24h at 180 ℃, naturally cooling to room temperature after the reaction is finished, washing the product to be neutral by distilled water, putting the product into a vacuum drying oven, vacuumizing to 0.01MPa, and heating for 24h at 80 ℃ to obtain rod-shaped potassium tantalate-niobate nano powder; the molar ratio of the tantalum pentoxide to the niobium pentoxide is 1:1, and the total molar amount of the tantalum pentoxide and the niobium pentoxide is 0.015 mol; the concentration of the potassium hydroxide aqueous solution is 8.5 mol/L; the molar ratio of the niobium pentoxide to the potassium hydroxide aqueous solution is 1: 68;
Secondly, uniformly mixing the rodlike potassium tantalate-niobate nano powder with a polyvinyl alcohol aqueous solution to obtain a mixture; pressing the mixture into a cylindrical sheet with the diameter of 12mm under the pressure of 10 MPa; putting the pressed cylindrical sheet into a muffle furnace, removing glue for 4h at the temperature of 550 ℃, and then sintering for 2h at the temperature of 1075-1125 ℃ to obtain the potassium tantalate-niobate ceramic with the ultrahigh dielectric constant; the mass fraction of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 8%; the mass ratio of the polyvinyl alcohol aqueous solution to the rodlike potassium tantalate niobate nano powder is 3: 100.
FIG. 1 is an X-ray diffraction pattern of the rod-shaped potassium tantalate-niobate nano powder obtained in the first step of the example; FIG. 2 is an X-ray diffraction diagram of a common potassium tantalate niobate nano-powder; it can be seen from fig. 1 and 2 that the diffraction peaks are both characteristic diffraction peaks of potassium tantalate niobate, which can indicate that no other impurity phase is generated in the prepared rodlike potassium tantalate niobate nano powder and the common potassium tantalate niobate nano powder, and that the synthesized product has high purity.
FIG. 3 is a scanning electron microscope image of the rod-shaped potassium tantalate-niobate nano powder obtained in the first step of the example; FIG. 4 is a scanning electron microscope image of a common potassium tantalate niobate nano powder; it can be clearly observed from the figure that the rod-shaped potassium tantalate niobate nano powder is rod-shaped, while the common potassium tantalate niobate nano powder is square.
FIG. 5 is a graph showing the dielectric spectrum of the ultra-high dielectric constant potassium tantalate-niobate ceramic obtained in step two of example; FIG. 6 is a graph of the dielectric spectrum of potassium tantalate niobate ceramic; from the comparison between FIG. 5 and FIG. 6, it can be clearly seen that the relative dielectric constant of the ceramic prepared from the rod-shaped potassium tantalate niobate nano powder is far higher than that of the ceramic prepared from the common potassium tantalate niobate nano powder in the frequency range of 40Hz to 106 Hz. At a frequency of 100Hz, the relative dielectric constant of the rod-shaped potassium tantalate-niobate ceramic is as high as 1.97X 104, while the relative dielectric constant of the common potassium tantalate-niobate ceramic is only 2.52X 103. The relative dielectric constant (2.81X 103) of the rod-shaped potassium tantalate-niobate ceramic is much higher than that (1.52X 103) of the common potassium tantalate-niobate ceramic even at a frequency of 106 Hz.
according to the method, the rod-shaped potassium tantalate-niobate nano powder is prepared by controlling the preparation process of a hydrothermal method, and then the rod-shaped potassium tantalate-niobate nano powder is used as a raw material to prepare the potassium tantalate-niobate ceramic with the ultrahigh dielectric constant. The new method for preparing the potassium tantalate niobate ceramic with the ultrahigh dielectric constant greatly widens the application of the potassium tantalate niobate ceramic in the field of dielectric materials.
Claims (7)
1. a preparation method of potassium tantalate niobate ceramic with an ultrahigh dielectric constant is characterized in that the preparation method of the potassium tantalate niobate ceramic with the ultrahigh dielectric constant is specifically carried out according to the following steps:
Firstly, preparing rod-shaped potassium tantalate-niobate powder: adding tantalum pentoxide and niobium pentoxide into a potassium hydroxide aqueous solution, magnetically stirring for 20-40 min, transferring to a hydrothermal reaction kettle, reacting for 20-30 h at 160-190 ℃, naturally cooling to room temperature after the reaction is finished, washing the product to be neutral by distilled water, putting the product into a vacuum drying oven, vacuumizing to 0.01MPa, and heating for 20-30 h at 60-85 ℃ to obtain rod-shaped potassium tantalate-niobate nano powder; the molar ratio of the tantalum pentoxide to the niobium pentoxide is 1: 1; the concentration of the potassium hydroxide aqueous solution is 8-9 mol/L; the molar ratio of the niobium pentoxide to the potassium hydroxide aqueous solution is 1 (60-70);
Secondly, uniformly mixing the rodlike potassium tantalate-niobate nano powder with a polyvinyl alcohol aqueous solution to obtain a mixture; pressing the mixture under 10Mpa to obtain cylindrical sheet with diameter of 12 mm; putting the pressed cylindrical sheet into a muffle furnace, removing glue for 4h at the temperature of 550 ℃, and then sintering for 2h at the temperature of 1075-1125 ℃ to obtain the potassium tantalate-niobate ceramic with the ultrahigh dielectric constant; the mass fraction of polyvinyl alcohol in the polyvinyl alcohol aqueous solution is 5-10%; the mass ratio of the polyvinyl alcohol aqueous solution to the rodlike potassium tantalate niobate nano powder is (1-10): 100.
2. the method for preparing potassium tantalate niobate ceramic with ultra-high dielectric constant as claimed in claim 1, wherein the reaction is carried out at 180 ℃ for 24h in step one.
3. The method for preparing potassium tantalate niobate ceramic with ultra-high dielectric constant as claimed in claim 1, wherein the heating is performed at 80 ℃ for 24h in step one.
4. The method for preparing potassium tantalate niobate ceramic with ultra-high dielectric constant as claimed in claim 1, wherein the concentration of the aqueous solution of potassium hydroxide in step one is 8.5 mol/L.
5. the method for preparing potassium tantalate niobate ceramic with ultra-high dielectric constant as claimed in claim 1, wherein the molar ratio of niobium pentoxide to aqueous solution of potassium hydroxide in step one is 1: 68.
6. the method for preparing potassium tantalate niobate ceramic with ultra-high dielectric constant as claimed in claim 1, wherein the mass fraction of polyvinyl alcohol in the polyvinyl alcohol aqueous solution in step two is 8%.
7. The method for preparing potassium tantalate niobate ceramic with ultra-high dielectric constant of claim 1, wherein the mass ratio of the polyvinyl alcohol aqueous solution to the rod-shaped potassium tantalate niobate nano powder in the second step is 3: 100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710400616.1A CN107176837B (en) | 2017-05-31 | 2017-05-31 | Preparation method of potassium tantalate niobate ceramic with ultrahigh dielectric constant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710400616.1A CN107176837B (en) | 2017-05-31 | 2017-05-31 | Preparation method of potassium tantalate niobate ceramic with ultrahigh dielectric constant |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107176837A CN107176837A (en) | 2017-09-19 |
| CN107176837B true CN107176837B (en) | 2019-12-06 |
Family
ID=59836306
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710400616.1A Expired - Fee Related CN107176837B (en) | 2017-05-31 | 2017-05-31 | Preparation method of potassium tantalate niobate ceramic with ultrahigh dielectric constant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107176837B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111747448A (en) * | 2020-07-06 | 2020-10-09 | 山东省科学院新材料研究所 | Preparation method of potassium tantalate niobate high-purity nanocrystal with adjustable forbidden band width |
| CN113683417A (en) * | 2021-08-19 | 2021-11-23 | 陕西天璇涂层科技有限公司 | Preparation method of nanocrystalline single-phase nickel niobate ceramic block |
| CN113773541A (en) * | 2021-10-08 | 2021-12-10 | 哈尔滨理工大学 | Preparation method of KTN/PI composite film with high breakdown and low dielectric loss |
| CN113956039B (en) * | 2021-11-30 | 2022-08-23 | 山东山科智晶光电科技有限公司 | Preparation method of large-size high-quality potassium tantalate niobate ceramic target |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786880A (en) * | 2010-02-11 | 2010-07-28 | 中国科学院上海硅酸盐研究所 | Sodium potassium niobate-potassium lithium niobate piezoelectric ceramics and preparation method thereof |
| CN103467096A (en) * | 2013-09-17 | 2013-12-25 | 河南科技大学 | Novel potassium sodium niobate-based leadless piezoelectric ceramics and preparation method thereof |
| CN105417580A (en) * | 2016-01-08 | 2016-03-23 | 哈尔滨理工大学 | Method for controlling potassium tantalate niobate nano powder size to be uniform through hydrothermal method |
| CN105601286A (en) * | 2015-12-18 | 2016-05-25 | 河海大学常州校区 | Erbium ytterbium-doped potassium lithium tantalite niobate ceramic and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2762462B1 (en) * | 2013-02-04 | 2020-12-23 | NXP USA, Inc. | Method of forming a target and depositing doped dielectric films by sputtering |
-
2017
- 2017-05-31 CN CN201710400616.1A patent/CN107176837B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786880A (en) * | 2010-02-11 | 2010-07-28 | 中国科学院上海硅酸盐研究所 | Sodium potassium niobate-potassium lithium niobate piezoelectric ceramics and preparation method thereof |
| CN103467096A (en) * | 2013-09-17 | 2013-12-25 | 河南科技大学 | Novel potassium sodium niobate-based leadless piezoelectric ceramics and preparation method thereof |
| CN105601286A (en) * | 2015-12-18 | 2016-05-25 | 河海大学常州校区 | Erbium ytterbium-doped potassium lithium tantalite niobate ceramic and preparation method thereof |
| CN105417580A (en) * | 2016-01-08 | 2016-03-23 | 哈尔滨理工大学 | Method for controlling potassium tantalate niobate nano powder size to be uniform through hydrothermal method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107176837A (en) | 2017-09-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107176837B (en) | Preparation method of potassium tantalate niobate ceramic with ultrahigh dielectric constant | |
| CN103508730B (en) | A kind of low sintering huge Jie's ceramic capacitor dielectric and preparation method thereof | |
| Chang et al. | Dielectric and piezoelectric properties of alkaline-earth titanate doped (K0. 5Na0. 5) NbO3 ceramics | |
| CN108275998A (en) | Ternary system PSN-PZT piezoelectric ceramic pieces and preparation method thereof | |
| CN111302797A (en) | Potassium-sodium niobate-based leadless piezoelectric ceramic and preparation method thereof | |
| CN103553605B (en) | KNN-BF leadless piezoelectric ceramic and preparation method thereof | |
| CN101774803B (en) | A (Ba, sr) TiO3-based ceramic medium and its prepn | |
| CN105036734A (en) | High-dielectric-constant X8R type dielectric material for multilayer porcelain capacitor, and preparation method for dielectric material | |
| CN104129988A (en) | Lead-free ceramic dielectric material with high energy storage density and high energy storage efficiency and preparation method thereof | |
| CN104529446A (en) | Copper oxide doped potassium-sodium niobate electrostrictive strain ceramic and preparation method thereof | |
| JPWO2009125681A1 (en) | Method for producing barium titanate | |
| CN104058741A (en) | Medium ceramic with stable ultra-wide temperature and preparation method thereof | |
| CN107032790B (en) | High-electromechanical conversion complex-phase piezoelectric ceramic material applied to energy collecting device and preparation method thereof | |
| CN113880576B (en) | Low sintering temperature and anisotropic strontium barium niobate sodium tungsten bronze type piezoelectric ferroelectric ceramic material and preparation method thereof | |
| CN115093216A (en) | Barium titanate doped lead-free ceramic with high electrostriction and low hysteresis and preparation method thereof | |
| CN101844919A (en) | Composite barium strontium titanate ceramics and preparation method thereof | |
| CN111217604B (en) | Preparation method of sodium bismuth titanate-based electronic ceramic with high energy storage density and efficiency | |
| CN103214241A (en) | Barium titanate-based lead-free piezoelectric luminous material and preparation method thereof | |
| CN106699177B (en) | Lead-free piezoelectric energy collecting material with high power generation characteristic and preparation method thereof | |
| CN111925209A (en) | Lead-free sound vibration piezoelectric transduction material and preparation method thereof | |
| CN111517788A (en) | Preparation method of potassium-sodium niobate ceramic material with high remanent polarization | |
| CN112062559B (en) | Antiferroelectric ceramic material and low-temperature sintering method thereof | |
| CN103864415B (en) | Barium titanate high dielectric ceramic of a kind of zinc doping and preparation method thereof | |
| CN103664168A (en) | Method for preparing BCTZ-xLa-system multifunctional electronic ceramic | |
| CN103435344B (en) | Piezoceramic material for high-frequency ceramic filter |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20191206 Termination date: 20200531 |