CN116283339A - Preparation method of pure-phase bismuth ferrite ceramic - Google Patents
Preparation method of pure-phase bismuth ferrite ceramic Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 77
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 36
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 33
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 51
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000005245 sintering Methods 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 43
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 26
- 239000013077 target material Substances 0.000 claims abstract description 14
- 239000012046 mixed solvent Substances 0.000 claims abstract description 13
- 239000011240 wet gel Substances 0.000 claims abstract description 12
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 10
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 230000005291 magnetic effect Effects 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 58
- 238000005303 weighing Methods 0.000 claims description 17
- 239000002994 raw material Substances 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000004570 mortar (masonry) Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 6
- 150000001768 cations Chemical class 0.000 claims description 5
- 239000000084 colloidal system Substances 0.000 claims description 5
- 238000005187 foaming Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 2
- 238000003980 solgel method Methods 0.000 abstract description 6
- 239000012071 phase Substances 0.000 description 20
- 238000002441 X-ray diffraction Methods 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 238000011160 research Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000005290 antiferromagnetic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000011214 refractory ceramic Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of functional ceramics, and discloses a preparation method of pure-phase bismuth ferrite ceramics. The preparation method comprises the following steps of dissolving bismuth nitrate pentahydrate, ferric nitrate nonahydrate and citric acid in a mixed solvent of anhydrous methanol and ethylene glycol; then placing the mixed solvent on a constant-temperature magnetic stirrer, heating and stirring to form wet gel, and drying in a drying oven; finally, drying and calcining the wet gel, and tabletting and sintering. The invention adopts a sol-gel method, ensures that all components are uniformly mixed, and definitely determines the pure phase BiFeO 3 The ceramic target material prepared by the method has high density, no generation of heterogeneous phase, simple equipment and preparation process, low cost and good repeatability.
Description
Technical Field
The invention relates to a preparation method of pure-phase bismuth ferrite ceramic, belonging to the technical field of functional ceramic.
Background
Bismuth ferrite is a rare multiferroic material with excellent ferroelectricity and antiferromagnetic property at room temperature, and because of the lead-free characteristic, bismuth ferrite has become one of the hot spots in the field of the current multiferroic material research, has wide application prospect in the fields of ferroelectric memories, photocatalytic degradation, high-temperature piezoelectric devices, energy storage dielectrics, ferroelectric photovoltaics and the like, and attracts a great deal of research interests of researchers.
Bismuth ferrite contains volatile element bismuth, and the preparation of the ceramic block is difficult to prepare pure-phase bismuth ferrite ceramic without impurity phases by common synthetic methods and sintering processes due to the factors of low sintering temperature, easy volatilization of bismuth element and the like, and the density is not satisfactory, thus the related research and application of bismuth ferrite are hindered. Common ceramic block preparation methods include a solid phase method, a hydrothermal method, a coprecipitation method, a sol-gel method and the like. The ceramic prepared by the solid phase method is often uneven in grain size, low in density and impure in phase formation, so that adverse effects are caused on subsequent application; the ceramic process prepared by the coprecipitation method is not easy to control, the repeatability is poor, the precipitant is easy to cause insufficient chemical reaction, so that local components are uneven, the particle size is different, mixed phases are generated, the reaction conditions (temperature, pressure and the like) of the hydrothermal method are strict, the ceramic process is not easy to control, the mixed phases are easy to generate in the processing process, and the synthesis temperature interval is narrow; the hydrothermal method requires high temperature and high pressure and long time in the preparation process, and the morphology control in the preparation process is difficult and impurities are easy to occur. The sol-gel method for preparing the ceramic material has the advantages of uniform raw material mixing, low sintering temperature, simple process and the like, and the method for preparing the bismuth ferrite film has a few researches, but is not seen in the preparation of bismuth ferrite ceramic blocks.
Therefore, based on the defects, the invention provides a sol-gel method for preparing single-phase bismuth ferrite ceramic, and a fine sintering system is matched, so that the problems of poor powder uniformity, low block density, impure phase formation and the like in the prior art are solved.
Disclosure of Invention
The invention aims to provide a preparation method for synthesizing pure-phase bismuth ferrite ceramic, which adopts a sol-gel method to prepare the bismuth ferrite ceramic, has the advantages of easy control of the preparation process, low sintering temperature and short time, and can effectively inhibit the generation of mixed phases and the volatilization of bismuth element serving as a reaction raw material. In addition, the method has the advantages of simple process, high efficiency, time saving, good repeatability, and low price and availability of the selected chemical reagent.
The preparation method of the pure-phase bismuth ferrite ceramic target material comprises the following steps:
(1) Calculating and weighing: calculated and weighed according to the chemical formula components, bismuth nitrate pentahydrate (Bi (NO 3 ) 3 ·5H 2 O), ferric nitrate nonahydrate (Fe (NO) 3 ) 3 ·9H 2 O) taking citric acid as an auxiliary raw material, accurately weighing the corresponding raw material, and controlling a certain weighing error;
(2) Preparing a solution: dissolving the bismuth nitrate pentahydrate, the ferric nitrate nonahydrate and the citric acid weighed in the step (1) in a mixed solvent of methanol and glycol, wherein the citric acid is used as a complexing agent, the glycol is used as a dispersing agent, and the mixed solvent is placed on a constant-temperature magnetic stirrer and stirred for a period of time to obtain a mixed solution;
(3) Colloid preparation: heating and stirring the mixed solution obtained in the step (2), evaporating the organic solvent methanol, and forming dark red wet gel after a period of time;
(4) And (3) foaming process: placing the wet gel into a drying box, and standing for a period of time to form xerogel;
(5) Preparation of presintered powder: taking the xerogel obtained in the step (4) out of a drying box, pouring the xerogel into a cleaned and dried agate mortar, and grinding for a period of time to obtain a certain amount of powder samples;
(6) Primary sintering process: uniformly pouring the powder obtained in the step (5) into a high-temperature-resistant ceramic crucible to compact a powder sample, then placing the ceramic crucible filled with the powder sample into a box-type furnace at a proper distance from a thermocouple for primary sintering, cooling the furnace to room temperature, taking out the powder sample, and preparing the primary sintered powder sample;
(7) The forming process comprises the following steps: taking out the primary calcined powder obtained in the step (6), putting the primary calcined powder into a cleaned and dried agate mortar, and grinding for a period of time; then weighing powder with certain mass, putting the powder into a proper mold, and pressurizing for a certain time under a certain pressure by using a tablet press to form a disc-shaped ceramic block;
(8) And (3) secondary sintering process: the BiFeO obtained in the step (7) is processed 3 Transferring the ceramic block into a high-temperature-resistant ceramic crucible, placing the ceramic crucible into a box-type furnace at a proper position away from a thermocouple, performing secondary calcination, reasonably setting sintering temperature and sintering time, cooling the furnace to room temperature, and taking out to obtain BiFeO 3 A ceramic target.
The weighing error of the step (1) is controlled within the range of +/-0.0005 g, and the citric acid and BiFeO are prepared 3 The molar ratio of metal cations is 1:1.
The volume ratio of the mixed solvent of the methanol and the glycol in the step (2) is 8:1-2:1.
The heating temperature of the mixed solution in the step (3) is 80-120 ℃ and the heating time is 0.5h.
The drying temperature of the oven in the step (4) is 120-140 ℃, the drying time is 8-12 h, and the drying atmosphere is normal pressure and air atmosphere.
The grinding time in the step (5) is 0.5-2 h.
The primary sintering temperature in the step (6) is 500-700 ℃, the heating time is 1.5-2.5 h, and the sintering atmosphere is normal pressure and air atmosphere.
In the step (7), the grinding time is 0.5-2 h, the powder quality is 1.5-15 g, the mould specification is 16-30 mm, the pressure of a tablet press is 1-2 Mpa, and the pressurizing time is 5-20 min.
The secondary calcination temperature in the step (8) is 850-900 ℃, the heating time is 1.5-2.5 h, and the sintering atmosphere is normal pressure and air atmosphere.
The invention has the beneficial effects that:
the method of the invention adopts a sol-gel method, so that the component elements can be mixed at an atomic level, the chemical components can be accurately controlled, and the ceramic block is uniform in phase formation; the required sintering temperature is low, the preparation process is easy to control, the particle size and the morphology of bismuth ferrite ceramic particles can be controlled, the problem of low density of blocks is overcome, and the generation of impurity phases is inhibited; the prepared bismuth ferrite ceramic target material is matched with an optimized sintering process system, has high density, uniform component and particle size distribution, no impurity phase and easy repetition, and lays a good foundation for the subsequent research of growing high-quality films, device preparation and the like by adopting a magnetron sputtering method or a pulse laser deposition method. Meanwhile, the method has the advantages of simple equipment and preparation process, high efficiency, time saving, low cost and good repeatability.
Drawings
FIG. 1 is an XRD pattern of a twice calcined sample of example 3;
FIG. 2 is an SEM photograph (500 times) of a twice calcined sample of example 3;
FIG. 3 is an XRD pattern for a twice calcined sample of example 4;
FIG. 4 is an SEM photograph (200 times) of a twice calcined sample of example 4;
FIG. 5 is an XRD pattern of a primary sintered powder sample of comparative example 1;
FIG. 6 is an XRD pattern of a twice calcined sample of comparative example 1;
FIG. 7 is an SEM photograph (300 times) of a twice calcined sample of comparative example 1;
FIG. 8 is an XRD pattern of a twice calcined sample of comparative example 2;
fig. 9 is an SEM photograph (500 x) of the twice calcined sample of comparative example 2.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific embodiments, but the scope of the invention is not limited to the description.
Example 1
The preparation method of the pure-phase bismuth ferrite ceramic target material specifically comprises the following steps:
(1) Calculating and weighing: calculated and weighed according to the chemical formula components, bismuth nitrate pentahydrate (Bi (NO 3 ) 3 ·5H 2 O), nitrate nonahydrateIron (Fe (NO) 3 ) 3 ·9H 2 O) is used as a raw material, citric acid is used as an auxiliary raw material, the corresponding raw material is accurately weighed, and the weighing error is controlled within a range of +/-0.0005 g, wherein, citric acid and BiFeO 3 The molar ratio of metal cations is 1:1;
(2) Preparing a solution: dissolving the bismuth nitrate pentahydrate, the ferric nitrate nonahydrate and the citric acid weighed in the step (1) in a mixed solvent of methanol and ethylene glycol, wherein the volume ratio of the mixed solvent of the methanol and the ethylene glycol is 2:1, and stirring uniformly by using a magnetic stirrer for a period of time to obtain a mixed solution;
(3) Colloid preparation: heating and stirring the mixed solution obtained in the step (2), wherein the heating temperature is 80 ℃, the heating time is 0.5h, and the organic solvent methanol is evaporated to form dark red wet gel after a period of time;
(4) And (3) foaming process: placing the wet gel into a drying box, wherein the drying temperature is 120 ℃, the drying time is 12 hours, and the drying atmosphere is normal pressure and air atmosphere to form xerogel;
(5) Preparation of presintered powder: taking the xerogel obtained in the step (4) out of a drying box, pouring the xerogel into a cleaned and dried agate mortar, and grinding for 0.5h to obtain a certain amount of powder samples;
(6) Primary sintering process: uniformly pouring the ceramic powder obtained in the step (5) into a high-temperature-resistant ceramic crucible to compact a powder sample, then placing the ceramic crucible filled with the powder sample into a box-type furnace to be positioned at a proper distance from a thermocouple for primary sintering, wherein the primary sintering temperature is 600 ℃, the heating time is 2.5h, the sintering atmosphere is normal pressure and air atmosphere, cooling the furnace to room temperature, taking out the powder sample, and finishing the preparation of the primary sintered powder sample;
(7) The forming process comprises the following steps: taking out the primary calcined powder obtained in the step (6), putting the primary calcined powder into a cleaned and dried agate mortar, grinding for 0.5h, then putting 1.5g of powder into a 16mm round die, and pressurizing for 5min under the pressure of 1Mpa by using a tablet press to form a disc-shaped ceramic block;
(8) And (3) secondary sintering process: the BiFeO obtained in the step (7) is processed 3 Transferring ceramics to a refractory ceramic cruciblePlacing the ceramic crucible in a box furnace at a proper position from a thermocouple, wherein the secondary calcination temperature is 850 ℃, the heating time is 1h, and the sintering atmosphere is normal pressure and air atmosphere, so as to obtain BiFeO 3 The test shows that the bismuth ferrite ceramic target prepared by the embodiment is relatively pure.
Example 2
The preparation method of the pure-phase bismuth ferrite ceramic target material specifically comprises the following steps:
(1) Calculating and weighing: calculated and weighed according to the chemical formula components, bismuth nitrate pentahydrate (Bi (NO 3 ) 3 ·5H 2 O), ferric nitrate nonahydrate (Fe (NO) 3 ) 3 ·9H 2 O) is used as a raw material, citric acid is used as an auxiliary raw material, the corresponding raw material is accurately weighed, and the weighing error is controlled within a range of +/-0.0005 g, wherein, citric acid and BiFeO 3 The molar ratio of metal cations is 1:1;
(2) Preparing a solution: dissolving the bismuth nitrate pentahydrate, the ferric nitrate nonahydrate and the citric acid weighed in the step (1) in a mixed solvent of methanol and ethylene glycol, wherein the volume ratio of the mixed solvent of the methanol and the ethylene glycol is 8:1, and stirring uniformly by using a magnetic stirrer for a period of time to obtain a mixed solution;
(3) Colloid preparation: heating and stirring the mixed solution obtained in the step (2), wherein the heating temperature is 120 ℃, the heating time is 0.5h, and the organic solvent methanol is evaporated to form dark red wet gel after a period of time;
(4) And (3) foaming process: placing the wet gel into a drying box, wherein the drying temperature is 140 ℃, the drying time is 8 hours, and the drying atmosphere is normal pressure and air atmosphere to form xerogel;
(5) Preparation of presintered powder: taking the xerogel obtained in the step (4) out of a drying box, pouring the xerogel into a cleaned and dried agate mortar, and grinding for 2 hours to obtain a certain amount of powder samples;
(6) Primary sintering process: uniformly pouring the ceramic powder obtained in the step (5) into a high-temperature-resistant ceramic crucible, then placing the ceramic crucible filled with the powder sample into a box-type furnace at a proper position away from a thermocouple, and performing primary sintering, wherein the primary sintering temperature is 700 ℃, the heating time is 1.5h, the sintering atmosphere is normal pressure and air atmosphere, the powder sample is taken out after the furnace temperature is cooled to room temperature, and the preparation of the primary sintering powder sample is completed;
(7) The forming process comprises the following steps: taking out the primary calcined powder obtained in the step (6), putting the powder into a cleaned and dried agate mortar, grinding for 2 hours, then putting 15g of the powder into a 30mm circular die, and pressurizing for 15 minutes under the pressure of 2Mpa by using a tablet press to form a circular ceramic block;
(8) And (3) secondary sintering process: the BiFeO obtained in the step (7) is processed 3 Transferring the ceramic into a high-temperature-resistant ceramic crucible, placing the ceramic crucible into a box furnace at a proper distance from a thermocouple, wherein the secondary calcination temperature is 850 ℃, the heating time is 2.5h, and the sintering atmosphere is normal pressure and air atmosphere to obtain BiFeO 3 The test shows that the bismuth ferrite ceramic target prepared by the embodiment is relatively pure.
Example 3
The preparation method of the pure-phase bismuth ferrite ceramic target material specifically comprises the following steps:
(1) Calculating and weighing: calculated and weighed according to the chemical formula components, bismuth nitrate pentahydrate (Bi (NO 3 ) 3 ·5H 2 O), ferric nitrate nonahydrate (Fe (NO) 3 ) 3 ·9H 2 O) is used as a raw material, citric acid is used as an auxiliary raw material, the corresponding raw material is accurately weighed, and the weighing error is controlled within a range of +/-0.0005 g, wherein, citric acid and BiFeO 3 The molar ratio of metal cations is 1:1;
(2) Preparing a solution: dissolving the bismuth nitrate pentahydrate, the ferric nitrate nonahydrate and the citric acid weighed in the step (1) in a mixed solvent of methanol and ethylene glycol, wherein the volume ratio of the mixed solvent of the methanol and the ethylene glycol is 3:1, and stirring uniformly by using a magnetic stirrer for a period of time to obtain a mixed solution;
(3) Colloid preparation: heating and stirring the mixed solution obtained in the step (2), wherein the heating temperature is 88 ℃, the heating time is 0.5h, and the organic solvent methanol is evaporated to form dark red wet gel after a period of time;
(4) And (3) foaming process: placing the wet gel into a drying box, wherein the drying temperature is 130 ℃, the drying time is 10 hours, and the drying atmosphere is normal pressure and air atmosphere to form xerogel;
(5) Preparation of presintered powder: taking the xerogel obtained in the step (4) out of a drying box, pouring the xerogel into a cleaned and dried agate mortar, and grinding for 1h to obtain a certain amount of powder sample;
(6) Primary sintering process: uniformly pouring the ceramic powder obtained in the step (5) into a high-temperature-resistant ceramic crucible, then placing the ceramic crucible filled with the powder sample into a box-type furnace at a proper position away from a thermocouple, and performing primary sintering, wherein the primary sintering temperature is 500 ℃, the heating time is 2h, the sintering atmosphere is normal pressure and air atmosphere, the powder sample is taken out after the furnace temperature is cooled to room temperature, and the preparation of the primary sintering powder sample is completed;
(7) The forming process comprises the following steps: taking out the primary calcined powder obtained in the step (6), putting the primary calcined powder into a cleaned and dried agate mortar, grinding for 1h, then putting 1.5g of powder into a 16mm round die, and pressurizing for 20min under the pressure of 1.5Mpa by using a tablet press to form a disc-shaped ceramic block;
(8) And (3) secondary sintering process: the BiFeO obtained in the step (7) is processed 3 Transferring the ceramic into a high-temperature-resistant ceramic crucible, placing the ceramic crucible into a box furnace at a proper distance from a thermocouple, wherein the secondary calcination temperature is 850 ℃, the heating time is 2 hours, and the sintering atmosphere is normal pressure and air atmosphere to obtain BiFeO 3 A ceramic target.
BiFeO prepared in this example 3 The XRD patterns of the ceramic targets are shown in figure 1, and can be seen to be relatively pure.
BiFeO prepared in this example 3 SEM photographs of the ceramic targets are shown in fig. 2.
Example 4
In this example, the temperature of the secondary sintering was 900 ℃, and the other steps and parameters were the same as in example 3.
BiFeO prepared in this example 3 The XRD patterns of the ceramic targets are shown in figure 3, and can be seen to be relatively pure.
Preparation of this exampleThe BiFeO obtained 3 SEM photographs of the ceramic targets are shown in fig. 4.
Comparative example 1
In this example, the temperature of the secondary sintering was 800℃and the other steps and parameters were the same as in example 3.
BiFeO prepared by primary sintering of powder sample in this example 3 The XRD pattern of the ceramic powder is shown in FIG. 5.
BiFeO prepared by secondary calcination in this example 3 The XRD pattern of the ceramic target is shown in figure 6, and a small amount of impurity phase is generated.
BiFeO prepared by secondary calcination in this example 3 SEM photographs of the ceramic targets are shown in fig. 7.
Comparative example 2
In this example, the temperature of the secondary sintering was 950 ℃, and the other steps and parameters were the same as in example 3.
BiFeO prepared in this example 3 As shown in FIG. 8, the XRD pattern of the ceramic powder has more impurity phases.
BiFeO prepared in this example 3 SEM photographs of the ceramic targets are shown in fig. 9.
Claims (9)
1. The preparation method of the pure-phase bismuth ferrite ceramic specifically comprises the following steps:
(1) Calculating and weighing: calculated and weighed according to the chemical formula components, bismuth nitrate pentahydrate (Bi (NO 3 ) 3 ·5H 2 O), ferric nitrate nonahydrate (Fe (NO) 3 ) 3 ·9H 2 O) taking citric acid as an auxiliary raw material, accurately weighing the corresponding raw material, and controlling a certain weighing error;
(2) Preparing a solution: dissolving the bismuth nitrate pentahydrate, the ferric nitrate nonahydrate and the citric acid weighed in the step (1) in a mixed solvent of methanol and ethylene glycol, and simultaneously stirring for a period of time by using a magnetic stirrer to obtain a mixed solution;
(3) Colloid preparation: heating and stirring the mixed solution obtained in the step (2), evaporating the organic solvent methanol, and forming wet gel after a period of time;
(4) And (3) foaming process: placing the wet gel into a drying box, and standing for a period of time at a certain temperature to form xerogel;
(5) Preparation of presintered powder: taking the xerogel obtained in the step (4) out of a drying box, pouring the xerogel into a mortar, and grinding for a period of time to obtain a certain amount of powder samples;
(6) Primary sintering process: uniformly pouring the powder obtained in the step (5) into a crucible to compact a powder sample, then placing the crucible filled with the powder sample into a box-type furnace for primary sintering, cooling the furnace to room temperature, taking out the powder sample, and completing the preparation of the primary sintered powder sample;
(7) The forming process comprises the following steps: taking out the primary calcined powder obtained in the step (6), putting the powder into a mortar, grinding for a period of time, weighing the powder with a certain mass, putting the powder into a proper mold, and pressurizing the powder for a certain time under a certain pressure by using a tablet press to form a disc-shaped ceramic block;
(8) And (3) secondary sintering process: transferring the bismuth ferrite block obtained in the step (7) into a high-temperature-resistant ceramic crucible, placing the ceramic crucible into a box-type furnace for secondary calcination, and taking out the ceramic crucible after the sintering is finished and the furnace temperature is cooled to room temperature, thus obtaining the bismuth ferrite ceramic target.
2. The method for preparing the pure-phase bismuth ferrite ceramic target material according to claim 1, which is characterized in that: the weighing error in the step (1) is controlled within the range of +/-0.0005 g, and citric acid and BiFeO are mixed 3 The molar ratio of metal cations is 1:1.
3. The method for preparing the pure-phase bismuth ferrite ceramic target material according to claim 1, which is characterized in that: the volume ratio of the mixed solvent of the methanol and the glycol in the step (2) is 8:1-2:1.
4. The method for preparing the pure-phase bismuth ferrite ceramic target material according to claim 1, which is characterized in that: the heating temperature of the mixed solution in the step (3) is 80-120 ℃, and the heating time period is 0.5h.
5. The method for preparing the pure-phase bismuth ferrite ceramic target material according to claim 1, which is characterized in that: the drying temperature of the oven in the step (4) is 120-140 ℃, the drying time is 8-12 h, and the drying atmosphere is normal pressure and air atmosphere.
6. The method for preparing the pure-phase bismuth ferrite ceramic target material according to claim 1, which is characterized in that: and (3) grinding for 0.5-2 h in the step (5).
7. The method for preparing the pure-phase bismuth ferrite ceramic target material according to claim 1, which is characterized in that: the primary sintering temperature in the step (6) is 500-700 ℃, the heating time is 1.5-2.5 h, and the sintering atmosphere is normal pressure and air atmosphere.
8. The method for preparing the pure-phase bismuth ferrite ceramic target material according to claim 1, which is characterized in that: and (3) grinding for 0.5-2 h in the step (7), weighing 1.5-15 g of powder, selecting a die with the specification of 16-30 mm, and using a tablet press for 1-2 Mpa and pressurizing for 5-20 min.
9. The method for preparing the pure-phase bismuth ferrite ceramic target material according to claim 1, which is characterized in that: the secondary calcination temperature in the step (8) is 850-900 ℃, the heating time is 1.5-2.5 h, and the sintering atmosphere is normal pressure and air atmosphere.
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