CN108558401B - Preparation of Bi by sol-gel method2/3Cu2Ta2Ti2O12Method for producing ceramic powder - Google Patents
Preparation of Bi by sol-gel method2/3Cu2Ta2Ti2O12Method for producing ceramic powder Download PDFInfo
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Abstract
The invention relates to a sol-gel method for preparing Bi2/ 3Cu2Ta2Ti2O12The method for preparing the ceramic powder mainly comprises the following steps: weighing anhydrous potassium carbonate and tantalum pentoxide, and putting the anhydrous potassium carbonate and the tantalum pentoxide into a cylindrical crucible for melting to obtain milky white frit; dissolving the milky white frit in deionized water, and gradually dropping nitric acid into the solution to generate hydrated Ta2O5White precipitate; then filtering, separating and washing the hydrated Ta2O5White precipitate for later use, hydrating Ta2O5Adding the solution into a citric acid aqueous solution, and dropwise adding a hydrogen peroxide solution to form a citric acid aqueous solution of clarified tantalum; weighing Bi (NO)3)3·5H2O、Cu(NO3)2·3H2O、Ti(C4H9O)4Adding Cu (NO)3)2·3H2Completely dissolving O in the citric acid aqueous solution of tantalum to form a solution 1; weighing ethylene glycol solution, and slowly dropwise adding Ti (C) into the ethylene glycol solution4H9O)4Adding Bi (NO) into the mixture3)3·5H2O, forming a solution 2; dropwise adding the solution 1 into the solution 2, and dropwise adding ammonia water to form gel; calcining and grinding to obtain Bi2/3Cu2Ta2Ti2O12Ceramic powder. Has the characteristics of fine and uniform particle size of powder particles, low synthesis temperature, good sintering crystallization performance, good sintering characteristic and the like.
Description
Technical Field
The invention belongs to the technical field of ceramic powder preparation processes, and relates to a sol-gel method for preparing Bi2/ 3Cu2Ta2Ti2O12A method for producing ceramic powder.
Background
The ceramic dielectric material is developed rapidly and has wide application prospect. The high dielectric ceramic material has the characteristics of high energy density, good dielectric property and temperature stability and the like, is a key material in the electronic industry, and is concerned. The high-performance ceramic capacitor prepared by taking the ceramic capacitor as a base material is a new-generation electronic component which is widely researched in recent years and is widely applied to the fields of national defense, detection, communication and the like: multilayer chip ceramic capacitors (MLCC) are prepared into resistors, PTC and NTC thermistors, and the demand is increasing; the resonator and the medium guided wave loop made of the microwave dielectric ceramic are widely applied to mobile communication of mobile phones, satellite receivers and the like, and have larger development space in scientific research and engineering application.
In the process of research and development of ceramic capacitor materials, ceramic materials having a perovskite-like structure are attracting attention. The material has low sintering temperature, obtains higher dielectric constant and smaller dielectric loss in a wide frequency range, can keep stable dielectric property at different temperatures, and does not generate ferroelectric phase transition to cause lattice distortion to cause performance deterioration. Meanwhile, perovskite-like structural materials also have many disadvantages: for example, under room temperature, the resistance changes with the voltage in a nonlinear way, the grain growth speed is too fast during sintering, the breakdown voltage is smaller, and the like. Therefore, aiming at the problems, the preparation process is changed, the root cause of the high dielectric response of the material is deeply researched, the dielectric loss and the dielectric nonlinearity are effectively reduced, the thermal stability and the electrical breakdown resistance are improved, and the method has important significance for researching and developing a novel perovskite-like ceramic capacitor material and popularizing the wide application of the perovskite-like ceramic capacitor material in the field of microelectronics.
Disclosure of Invention
In order to overcome the above disadvantages of the prior art, the present invention provides a sol-gel method for preparing Bi2/3Cu2Ta2Ti2O12The method for preparing the ceramic powder has the characteristics of fine and uniform powder particle size, low synthesis temperature, good sintering crystallization performance, good sintering characteristic and the like, and simultaneously, the preparation raw materials have wide sources, are easy to operate and have no impurities.
The technical scheme adopted by the invention for solving the technical problems is as follows: preparation of Bi by sol-gel method2/ 3Cu2Ta2Ti2O12The method for preparing the ceramic powder mainly comprises the following steps:
(1) accurately weighing anhydrous potassium carbonate and tantalum pentoxide according to a molar ratio of 4.5-7: 1, uniformly mixing, putting into a cylindrical crucible, and melting in a muffle furnace at 850-950 ℃ for 3-8 hours to obtain a milky frit;
(2) dissolving the milky white frit obtained in the step (1) in 500mL of deionized water, standing for 6-12 hours, taking out the upper clear solution by using a suction tube, gradually dropping nitric acid into the solution, adjusting the pH value of the solution to 2-3, and ensuring that all hydrated Ta is generated2O5White precipitate;
(3) filtering, separating and washing the hydrated Ta in the step (2)2O5White precipitate is reserved, and the molar ratio of citric acid to total metal cations is 1-4: 1 preparing citric acid aqueous solution accurately, and then hydrating Ta2O5Adding into citric acid water solution, adding hydrogen peroxide solution, heating in water bath, stirring to hydrate Ta2O5Completely dissolving to form a citric acid aqueous solution of clarified tantalum;
(4) according to the formula Bi2/3Cu2Ta2Ti2O12Separately weighing Bi (NO)3)3·5H2O、Cu(NO3)2·3H2O、Ti(C4H9O)4Adding Cu (NO)3)2·3H2Dissolving O in citric acid aqueous solution of tantalum completely, heating in water bath, and stirring to clarify to form solution 1;
(5) weighing an ethylene glycol solution according to the molar ratio of ethylene glycol to citric acid of 1-3: 1, and slowly dropwise adding Ti (C)4H9O)4Continuously stirring and mixing for 30 minutes, and then adding Bi (NO)3)3·5H2O, continuously stirring and mixing for 1 hour to form a solution 2;
(6) slowly dripping the solution 1 into the solution 2, fully stirring and mixing for 20-30 minutes, then dripping ammonia water, adjusting the pH value to 6-7, heating in a water bath, stirring and reacting for 6-10 hours to form gel;
(7) drying the obtained gel, calcining and grinding to obtain Bi2/3Cu2Ta2Ti2O12Ceramic powder.
Step (3) hydration of Ta2O5Washing the white precipitate for 6-8 times, wherein the pH value of the liquid after suction filtration is 7-8.
The molar ratio of the hydrogen peroxide solution to the citric acid in the step (3) is 2-3: 1.
the water bath heating temperature of the steps (3), (4) and (6) is 65-85 ℃.
The drying temperature in the step (7) is 90-150 ℃, and the drying time is 4-30 hours; the calcination system is as follows: and (3) heating the dried sample to 500-800 ℃ from room temperature at the speed of 2-4 ℃/min, preserving the heat for 4-10 hours, and cooling along with the furnace.
The invention has the positive effects that: with anhydrous K2CO3、Ta2O5、Bi(NO3)3·5H2O、Cu(NO3)2·3H2O、Ti(C4H9O)4And citric acid is used as a raw material, ethylene glycol is used as a solvent, and a sol-gel method is utilized to prepare Bi with uniform particle size and good crystallization property2/3Cu2Ta2Ti2O12The ceramic powder is tested and analyzed by an XRD diffractometer and a scanning electron microscope, the powder synthesized by the method has fine and uniform particles, the average particle size is about 0.5-2 mu m, the crystallization performance is good, the sintering characteristic is good, and meanwhile, the preparation raw materials are wide in source, easy to operate and free of impurities.
Drawings
FIG. 1 is a diagram of a DSC-TG of a xerogel prepared according to the present invention.
FIG. 2 is an XRD pattern of the ceramic powder after 500-800 ℃ calcination of the xerogel prepared by the invention.
FIG. 3 is an SEM image of a ceramic powder after calcination at 800 ℃ of a xerogel prepared by the present invention.
Detailed Description
The invention is further explained below with reference to the drawings and the embodiments.
Example 1
Preparation of Bi by sol-gel method2/3Cu2Ta2Ti2O12The method for preparing the ceramic powder comprises the following steps:
(1) accurately weighing anhydrous potassium carbonate and tantalum pentoxide according to a molar ratio of 5:1, uniformly mixing, putting into a cylindrical crucible, and melting at 900 ℃ for 4 hours in a muffle furnace to obtain the milky white frit.
(2) Dissolving the milky white frit obtained in the step (1) in 500mL of deionized water, standing for 8 hours, taking out the upper clear solution by using a suction tube, gradually dropping nitric acid into the solution, adjusting the pH value to 2 and ensuring that all hydrated Ta is generated2O5White precipitate.
(3) Filtering, separating and washing (2) hydrated Ta2O5The white precipitate is reserved for 6 times, the pH of the liquid after suction filtration is 7, and the ratio of citric acid to total metal cations is 1.5:1 preparing citric acid aqueous solution accurately, and then hydrating Ta2O5Adding the mixture into a citric acid aqueous solution, and dropwise adding a hydrogen peroxide solution, wherein the molar ratio of the hydrogen peroxide solution to the citric acid is 2:1, heating in 75 ℃ water bath, stirring to hydrate Ta2O5Completely dissolved to form a citric acid aqueous solution of clarified tantalum.
(4) According to the formula Bi2/3Cu2Ta2Ti2O12Separately weighing Bi (NO)3)3·5H2O、Cu(NO3)2·3H2O、Ti(C4H9O)4Adding Cu (NO)3)2·3H2And completely dissolving O in the citric acid aqueous solution of tantalum, heating in a water bath at 80 ℃, and stirring until the solution is clear to form a solution 1.
(5) Weighing ethylene glycol solution according to the molar ratio of the ethylene glycol to the citric acid of 1.5:1, and slowly dropwise adding Ti (C)4H9O)4Continuously stirring and mixing for 30 minutes, and then adding Bi (NO)3)3·5H2O, continue to mix for 1 hour with stirring to form solution 2.
(6) And slowly dropwise adding the solution 1 into the solution 2, fully stirring and mixing for 20 minutes, then dropwise adding ammonia water, adjusting the pH value to 6, heating in a water bath at 80 ℃, stirring and reacting for 6 hours to form gel.
(7) Drying the gel at 110 deg.C for 6 hr, calcining the dried sample, heating to 500 deg.C at 2 deg.C/min, and heating to 600 deg.CKeeping the temperature at 700 ℃ and 800 ℃ for 8 hours, cooling along with the furnace, and grinding to obtain Bi2/3Cu2Ta2Ti2O12Ceramic powder.
For prepared Bi2/3Cu2Ta2Ti2O12The ceramic powder is tested, and the specific test conditions are as follows:
the xerogel is thermally analyzed by a comprehensive thermal analyzer (DSC-TG), and as can be seen from figure 1, the chemical reaction and the weight loss are completed before 500 ℃; the phase analysis of the ceramic powder after the xerogel is calcined at the temperature of 500-800 ℃ is carried out by XRD diffraction, and as can be seen from figure 2, the main phase of the prepared powder is Cu3Ta2Ti2O12(JCPDS #70-0610) and further comprises, for example, TiO2Bismuth titanium oxide and other small amount of mixed phases with good crystallization performance; the appearance of the ceramic powder after the xerogel is calcined at 800 ℃ is observed by adopting a Scanning Electron Microscope (SEM), and Bi can be seen from figure 32/3Cu2Ta2Ti2O12The ceramic powder has fine and uniform particles, the average particle size is about 0.5-2 mu m, and no obvious agglomeration phenomenon.
Example 2
Preparation of Bi by sol-gel method2/3Cu2Ta2Ti2O12The method for preparing the ceramic powder comprises the following steps:
(1) accurately weighing anhydrous potassium carbonate and tantalum pentoxide according to a molar ratio of 6:1, uniformly mixing, putting into a cylindrical crucible, and melting at 920 ℃ for 6 hours in a muffle furnace to obtain milky white frit.
(2) Dissolving the milky white frit obtained in the step (1) in 500mL of deionized water, standing for 10 hours, taking out the upper clear solution by using a suction tube, gradually dropping nitric acid into the solution, adjusting the pH value to 2 and ensuring that all hydrated Ta is generated2O5White precipitate.
(3) Filtering, separating and washing (2) hydrated Ta2O5The white precipitate is reserved for 8 times, the pH of the liquid after suction filtration is 7, and the molar ratio of citric acid to total metal cations is 2:1 preparing the citric acid aqueous solution accuratelyThen hydrate Ta2O5Adding the mixture into a citric acid aqueous solution, and dropwise adding a hydrogen peroxide solution, wherein the molar ratio of the hydrogen peroxide solution to the citric acid is 2.5: 1, heating in water bath at 80 ℃, stirring to hydrate Ta2O5Completely dissolved to form a citric acid aqueous solution of clarified tantalum.
(4) According to the formula Bi2/3Cu2Ta2Ti2O12Separately weighing Bi (NO)3)3·5H2O、Cu(NO3)2·3H2O、Ti(C4H9O)4Adding Cu (NO)3)2·3H2And completely dissolving O in the citric acid aqueous solution of tantalum, heating in a water bath at 85 ℃, and stirring until the solution is clear to form a solution 1.
(5) Weighing ethylene glycol solution according to the molar ratio of the ethylene glycol to the citric acid of 2:1, and slowly dropwise adding Ti (C)4H9O)4Continuously stirring and mixing for 30 minutes, and then adding Bi (NO)3)3·5H2O, continue to mix for 1 hour with stirring to form solution 2.
(6) And slowly dropwise adding the solution 1 into the solution 2, fully stirring and mixing for 25 minutes, then dropwise adding ammonia water, adjusting the pH value to 7, heating in a water bath at 80 ℃, stirring and reacting for 8 hours to form gel.
(7) Drying the obtained gel at 130 ℃ for 8 hours, then calcining the dried sample, heating to 750 ℃ at the speed of 3 ℃/min, preserving heat for 8 hours, cooling along with the furnace, and grinding to obtain Bi2/3Cu2Ta2Ti2O12Ceramic powder.
Example 3
Preparation of Bi by sol-gel method2/3Cu2Ta2Ti2O12The method for preparing the ceramic powder comprises the following steps:
(1) accurately weighing anhydrous potassium carbonate and tantalum pentoxide according to a molar ratio of 7:1, uniformly mixing, putting into a cylindrical crucible, and melting in a muffle furnace at 950 ℃ for 8 hours to obtain a milky white frit.
(2) Dissolving the milky white frit obtained in the step (1)Dissolving in 500mL deionized water, standing for 12 hr, taking out the upper clear solution with a straw, gradually dropping nitric acid into the solution, adjusting pH to 3 to ensure that all hydrated Ta is generated2O5White precipitate.
(3) Filtering, separating and washing (2) hydrated Ta2O5The white precipitate is reserved for 8 times, the pH of the liquid after suction filtration is 8, and the ratio of citric acid to total metal cations is 4: 1 preparing citric acid aqueous solution accurately, and then hydrating Ta2O5Adding the mixture into a citric acid aqueous solution, and dropwise adding a hydrogen peroxide solution, wherein the molar ratio of the hydrogen peroxide solution to the citric acid is 3:1, heating in water bath at 85 ℃, stirring to hydrate Ta2O5Completely dissolved to form a citric acid aqueous solution of clarified tantalum.
(4) According to the formula Bi2/3Cu2Ta2Ti2O12Separately weighing Bi (NO)3)3·5H2O、Cu(NO3)2·3H2O、Ti(C4H9O)4Adding Cu (NO)3)2·3H2And completely dissolving O in the citric acid aqueous solution of tantalum, heating in a water bath at 80 ℃, and stirring until the solution is clear to form a solution 1.
(5) Weighing ethylene glycol solution according to the molar ratio of ethylene glycol to citric acid of 3:1, and slowly dropwise adding Ti (C)4H9O)4Continuously stirring and mixing for 30 minutes, and then adding Bi (NO)3)3·5H2O, continue to mix for 1 hour with stirring to form solution 2.
(6) And slowly dropwise adding the solution 1 into the solution 2, fully stirring and mixing for 30 minutes, then dropwise adding ammonia water, adjusting the pH value to 7, heating in a water bath at 80 ℃, stirring and reacting for 10 hours to form gel.
(7) Drying the obtained gel at 150 ℃ for 12 hours, then calcining the dried sample, heating to 650 ℃ at the speed of 4 ℃/min, preserving heat for 10 hours, cooling along with the furnace, and grinding to obtain Bi2/3Cu2Ta2Ti2O12Ceramic powder.
Claims (5)
1. Preparation of Bi by sol-gel method2/3Cu2Ta2Ti2O12The method for preparing the ceramic powder is characterized by mainly comprising the following steps of:
(1) accurately weighing anhydrous potassium carbonate and tantalum pentoxide according to a molar ratio of 4.5-7: 1, uniformly mixing, putting into a cylindrical crucible, and melting in a muffle furnace at 850-950 ℃ for 3-8 hours to obtain a milky frit;
(2) dissolving the milky white frit obtained in the step (1) in 500mL of deionized water, standing for 6-12 hours, taking out the upper clear solution by using a suction tube, gradually dropping nitric acid into the solution, adjusting the pH value of the solution to 2-3, and ensuring that all hydrated Ta is generated2O5White precipitate;
(3) filtering, separating and washing the hydrated Ta in the step (2)2O5White precipitate is reserved, and the molar ratio of citric acid to total metal cations is 1-4: 1 preparing citric acid aqueous solution accurately, and then hydrating Ta2O5Adding into citric acid water solution, adding hydrogen peroxide solution, heating in water bath, stirring to hydrate Ta2O5Completely dissolving to form a citric acid aqueous solution of clarified tantalum;
(4) according to the formula Bi2/3Cu2Ta2Ti2O12Separately weighing Bi (NO)3)3·5H2O、Cu(NO3)2·3H2O、Ti(C4H9O)4Adding Cu (NO)3)2·3H2Dissolving O in citric acid aqueous solution of tantalum completely, heating in water bath, and stirring to clarify to form solution 1;
(5) weighing an ethylene glycol solution according to the molar ratio of ethylene glycol to citric acid of 1-3: 1, and slowly dropwise adding Ti (C)4H9O)4Continuously stirring and mixing for 30 minutes, and then adding Bi (NO)3)3·5H2O, continuously stirring and mixing for 1 hour to form a solution 2;
(6) slowly dripping the solution 1 into the solution 2, fully stirring and mixing for 20-30 minutes, then dripping ammonia water, adjusting the pH value to 6-7, heating in a water bath, stirring and reacting for 6-10 hours to form gel;
(7) drying the obtained gel, calcining and grinding to obtain Bi2/3Cu2Ta2Ti2O12Ceramic powder.
2. The sol-gel method of claim 1 for preparing Bi2/3Cu2Ta2Ti2O12The method for preparing the ceramic powder is characterized by comprising the following steps: step (3) hydration of Ta2O5Washing the white precipitate for 6-8 times, wherein the pH value of the liquid after suction filtration is 7-8.
3. The sol-gel method of claim 1 for preparing Bi2/3Cu2Ta2Ti2O12The method for preparing the ceramic powder is characterized by comprising the following steps: the molar ratio of the hydrogen peroxide solution to the citric acid in the step (3) is 2-3: 1.
4. the sol-gel method of claim 1 for preparing Bi2/3Cu2Ta2Ti2O12The method for preparing the ceramic powder is characterized by comprising the following steps: the water bath heating temperature of the steps (3), (4) and (6) is 65-85 ℃.
5. The sol-gel method of claim 1 for preparing Bi2/3Cu2Ta2Ti2O12The method for preparing the ceramic powder is characterized by comprising the following steps: the drying temperature in the step (7) is 90-150 ℃, and the drying time is 4-30 hours; the calcination system is as follows: and (3) heating the dried sample to 500-800 ℃ from room temperature at the speed of 2-4 ℃/min, preserving the heat for 4-10 hours, and cooling along with the furnace.
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| CN201810472207.7A CN108558401B (en) | 2018-05-17 | 2018-05-17 | Preparation of Bi by sol-gel method2/3Cu2Ta2Ti2O12Method for producing ceramic powder |
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| CN108558401B true CN108558401B (en) | 2021-08-17 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531528A (en) * | 2009-04-13 | 2009-09-16 | 天津大学 | Method for preparing magnesium niobate microwave ceramic powder on the basis of sol-gel technique |
| CN104609860A (en) * | 2015-01-25 | 2015-05-13 | 济南唯博新材料有限公司 | Preparation for magnesium niobate microwave ceramic powder through sol-gel technology |
| CN104609466A (en) * | 2015-01-25 | 2015-05-13 | 济南唯博新材料有限公司 | Method for finely synthesizing ilmenite-structured ZnTiO3 nano powder by using water-soluble sol-gel process |
| CN104609861A (en) * | 2015-01-25 | 2015-05-13 | 济南唯博新材料有限公司 | Method for fine synthesis of Ba(Zn1/3Nb2/3)O3 dielectric ceramic nano-powder through utilizing water-soluble sol-gel method |
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| JP4398635B2 (en) * | 2002-09-24 | 2010-01-13 | 株式会社ノリタケカンパニーリミテド | Piezoelectric ceramics |
| CN100548919C (en) * | 2007-06-21 | 2009-10-14 | 山东大学 | A kind of low temperature prepares Bi 3TiNbO 9The method of micro-nano piezoelectricity ferro powder |
| CN101774812B (en) * | 2010-02-02 | 2012-05-09 | 天津大学 | Method for preparing magnesium tantalate microwave ceramic powder by sol-gel technique |
| CN101921112A (en) * | 2010-07-06 | 2010-12-22 | 齐齐哈尔大学 | Sol-gel method for preparing potassium-sodium niobate nano-powder |
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| CN103708834A (en) * | 2013-05-24 | 2014-04-09 | 济南大学 | New method for finely preparing ixiolite structure MgTiNb2O8 microwave dielectric ceramic by using chemical process |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531528A (en) * | 2009-04-13 | 2009-09-16 | 天津大学 | Method for preparing magnesium niobate microwave ceramic powder on the basis of sol-gel technique |
| CN104609860A (en) * | 2015-01-25 | 2015-05-13 | 济南唯博新材料有限公司 | Preparation for magnesium niobate microwave ceramic powder through sol-gel technology |
| CN104609466A (en) * | 2015-01-25 | 2015-05-13 | 济南唯博新材料有限公司 | Method for finely synthesizing ilmenite-structured ZnTiO3 nano powder by using water-soluble sol-gel process |
| CN104609861A (en) * | 2015-01-25 | 2015-05-13 | 济南唯博新材料有限公司 | Method for fine synthesis of Ba(Zn1/3Nb2/3)O3 dielectric ceramic nano-powder through utilizing water-soluble sol-gel method |
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