CN114057482A - Sodium bismuth titanate-based ferroelectric ceramic gel-casting preparation method - Google Patents
Sodium bismuth titanate-based ferroelectric ceramic gel-casting preparation method Download PDFInfo
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Abstract
The invention discloses a bismuth sodium titanate-based ferroelectric ceramic gel-casting preparation method, which comprises the following steps: dissolving an organic monomer acrylamide and a cross-linking agent N, N' -methylene bisacrylamide in water according to a mass ratio of 12: 1-24: 1 to obtain a premixed solution with a concentration of 5-20 wt.%; adding sodium bismuth titanate-based ceramic powder and a dispersing agent into the premixed liquid, wherein the mass of the dispersing agent is 1-8 wt% of that of the ceramic powder, and the solid content of the ceramic powder is 40-60 vol%; adding an initiator solution with the concentration of 1-8% of a catalyst and the solution into the suspension solution to obtain ceramic slurry, wherein the mass ratio of the initiator to the premixed solution is 5-30 wt%, and the mass ratio of the catalyst to the premixed solution is 1-10 wt%; injecting the ceramic slurry into a mold for curing to obtain a ceramic blank; drying the embryo body in the environment with the temperature of 15-20 ℃ and the humidity of 80-90%; the blank body is degummed at the environmental heating rate of 0.3 ℃/min to 0.5 ℃/min, and the ceramic sintering is carried out at the temperature of 1030 ℃ to 1080 ℃. The method can effectively control the agglomeration of particles, and prepare the ceramic with uniform components, good compactness, large size and complex shape.
Description
Technical Field
The invention belongs to the technical field of electronic ceramic forming, and particularly relates to a sodium bismuth titanate-based ferroelectric ceramic gel-casting preparation method.
Background
Ferroelectric ceramic materials are widely used in the fields of electronics, machinery, medical treatment, etc. due to their unique electrical characteristics. At present, the common industrial preparation method of the block ceramic mainly adopts dry pressing, and the dry pressing is difficult to uniformly fill a mold and press due to poor ceramic powder flowability, and blank compact density or forming pressure distribution has fluctuation, so that the components of the block ceramic are uneven and the physical properties are poor.
Disclosure of Invention
Aiming at the defects or the improvement requirements of the prior art, the invention provides a bismuth sodium titanate-based ferroelectric ceramic gel injection molding preparation method, which aims to solve the technical problem of poor performance of ceramics obtained by dry pressing.
In order to achieve the above object, according to one aspect of the present invention, there is provided a bismuth sodium titanate-based ferroelectric ceramic gel-casting preparation method, comprising:
preparing a premixed solution: weighing an organic monomer acrylamide and a cross-linking agent N, N '-methylene bisacrylamide according to a mass ratio of 12: 1-24: 1, and dissolving the organic monomer acrylamide and the cross-linking agent N, N' -methylene bisacrylamide in water to obtain a premixed solution with a concentration of 5-20 wt.%;
preparation of suspension solutions: adding sodium bismuth titanate-based ceramic powder and a dispersing agent into the premixed liquid, wherein the mass of the dispersing agent is 1-8 wt% of that of the ceramic powder, and the solid content of the ceramic powder is controlled to be 40-60 vol%;
initiator and catalyst addition: adding an initiator solution with the concentration of 1-8% of a catalyst and the solution into the suspension solution and stirring to obtain ceramic slurry, wherein the mass ratio of the initiator to the premixed solution is 5-30 wt%, and the mass ratio of the catalyst to the premixed solution is 1-10 wt%;
and (3) injection molding and curing: injecting the ceramic slurry into a mold for curing to obtain a ceramic blank;
drying the blank: drying the ceramic blank body in an environment with the temperature of 15-20 ℃ and the humidity of 80-90%;
and (3) blank glue discharging: regulating the heating rate to be 0.3-0.5 ℃/min, heating to 600 ℃, preserving the heat for 1-2 h, and cooling;
and (3) sintering of ceramics: the sintering temperature is 1030-1080 ℃, and the heat preservation time is 2-3 h.
Preferably, when the suspension solution is prepared, a ball milling tank is used as a container, and the premixed liquid, the sodium bismuth titanate-based ceramic powder and the dispersing agent are poured into the ball milling tank and ball milled to obtain the suspension solution.
Preferably, the dispersant comprises polymethacrylic acid amine or citric acid amine.
Preferably, the initiator solution is an ammonium persulfate solution.
Preferably, the catalyst is N, N' -tetramethylethylenediamine.
Preferably, the adding the catalyst and the initiator solution with the solution concentration of 1-8% into the suspension solution and stirring comprises,
and transferring the suspension solution into a beaker, adding the initiator solution and the catalyst, and carrying out magnetic stirring in a vacuum state to carry out vacuum defoaming for 10-50 min.
Preferably, the mold is left at room temperature for 12 to 24 hours to cure the ceramic slurry while performing the injection molding curing.
Preferably, the step of drying the green body comprises:
placing the ceramic blank in an environment with the temperature of 15-20 ℃ and the humidity of 80-90%, and drying for 3-5 days;
adjusting the humidity to 40% -60%, and drying for 1-2 days;
transferring the mixture to an oven with the temperature of 60-80 ℃ for baking for 30-60 min.
Preferably, when the embryo body is subjected to rubber discharge, the embryo body is placed in a muffle furnace for rubber discharge.
The bismuth sodium titanate-based ferroelectric ceramic is prepared by using a gel casting technology, ceramic powder, a dispersing agent, a solvent and other ingredients are mixed in a liquid state, and then a blank body with a certain shape is obtained by removing the solvent and other methods, so that the agglomeration of particles can be effectively controlled, and a ceramic part with uniform components, good compactness, large size and complex shape is prepared. Compared with the traditional dry pressing, the agglomeration of ceramic particles can be effectively controlled by the gel injection molding technology, and the components are uniform in the ceramic forming process and the sintering process, so that the ceramic performance fluctuation caused by the nonuniform structure is avoided, and the stability and the reliability of the ceramic performance are improved.
Drawings
FIG. 1 is a flow chart of the steps of a gel-casting method for preparing a sodium bismuth titanate-based ferroelectric ceramic according to an embodiment of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Fig. 1 is a flow chart illustrating steps of a gel injection molding method for preparing a sodium bismuth titanate-based ferroelectric ceramic according to an embodiment of the present application, the method including:
step S100: preparing a premixed solution: the method comprises the steps of weighing an organic monomer acrylamide and a cross-linking agent N, N '-methylene bisacrylamide according to a mass ratio of 12: 1-24: 1, and dissolving the organic monomer acrylamide and the cross-linking agent N, N' -methylene bisacrylamide in water to obtain a premixed solution with a concentration of 5-20 wt.%.
Step S200: preparation of suspension solutions: and adding sodium bismuth titanate-based ceramic powder and a dispersing agent into the premixed liquid, wherein the mass of the dispersing agent is 1-8 wt% of that of the ceramic powder, and the solid content of the ceramic powder is controlled to be 40-60 vol%.
In an embodiment, a ball milling tank is used as a container, a certain amount of the premixed liquid prepared in step S100 is added into the ball milling tank, a certain amount of the sodium bismuth titanate-based ceramic powder is weighed, and in order to uniformly disperse the ceramic powder, the sodium bismuth titanate-based ceramic powder and a dispersant of a corresponding mass are added into the premixed liquid for multiple times to obtain a slurry of a corresponding solid content. Wherein, the solid content of the ceramic powder in the slurry is kept between 40 vol.% and 60 vol.%, and the dosage of the dispersant is 1 wt.% to 8 wt.% of the mass of the ceramic powder. Ball milling to obtain suspension solution with good flowability. Specifically, the dispersant may be selected from ammonium polymethacrylate, ammonium citrate, and the like.
Step S300: initiator and catalyst addition: adding an initiator solution with the concentration of 1-8% of a catalyst and the solution into the suspension solution and stirring to obtain the ceramic slurry, wherein the mass ratio of the initiator to the premixed solution is 5-30 wt%, and the mass ratio of the catalyst to the premixed solution is 1-10 wt%.
In one embodiment, the initiator may be composed of ammonium persulfate. A certain mass of ammonium persulfate solid can be weighed firstly and dissolved in deionized water to prepare an initiator solution with the solution concentration of 1-8%.
In one embodiment, the suspension solution prepared in step S200 is transferred to a beaker, the prepared initiator solution and catalyst are added, and magnetic stirring is performed under vacuum. Specifically, the catalyst can be N, N, N '-Tetramethylethylenediamine (TEMED), the addition amount of the initiator accounts for 5 wt% to 30 wt%, the addition amount of the catalyst N, N, N' -Tetramethylethylenediamine (TEMED) accounts for 1 wt% to 10 wt%, and the vacuum defoaming time is 10 to 50 min.
Step S400: and (3) injection molding and curing: and injecting the ceramic slurry into a mold for curing to obtain a ceramic blank.
And (5) slowly injecting the ceramic slurry obtained in the step (S300) into the mold along the mold wall, and sealing the mold opening with a preservative film in time after injection molding is finished to prevent pollution. And standing the die for 12-24 hours at room temperature to ensure that the slurry is solidified.
Step S500: drying the blank: the ceramic blank is dried in an environment with the temperature of 15-20 ℃ and the humidity of 80-90 percent.
Wherein, the drying of the embryo body specifically comprises: placing the solidified blank in a stable environment, adjusting the temperature to be 15-20 ℃ and the humidity to be 80-90%, and drying for 3-5 days; and adjusting the temperature to 15-20 ℃, the humidity to 40-60%, drying for 1-2 days, and indicating that the moisture in the blank body is basically removed when the quality of the blank body does not change. And baking the mixture in a baking oven at the temperature of between 60 and 80 ℃ for 30 to 60min to completely dry the mixture.
Step S600: and (3) blank glue discharging: regulating the heating rate to 0.3-0.5 ℃/min, heating to 600 ℃, preserving the temperature for 1-2 h, and cooling.
Specifically, the blank glue discharging comprises the steps of putting a dried blank into a muffle furnace, heating to 600 ℃ at the heating rate of 0.3-0.5 ℃/min, preserving heat for 1-2 hours, and then cooling along with the furnace.
Step S700: and (3) sintering of ceramics: the sintering temperature is 1030-1080 ℃, and the heat preservation time is 2-3 h.
Specifically, the ceramic sintering comprises sintering the blank in a muffle furnace, wherein the sintering temperature is 1030-1080 ℃, and the heat preservation time is 2-3 h.
And drying the blank, removing the glue from the blank and sintering the ceramic to obtain the sodium bismuth titanate-based ferroelectric ceramic.
In order to further understand the present invention, the following description will be given with specific examples.
Example 1
0.97 (Bi) is prepared by adopting gel injection molding technology0.5Na0.5)TiO3-0.03Ba(Nb0.5Ni0.5)O3A ferroelectric ceramic.
With Bi2O3、NaHCO3、TiO2、BaCO3、Nb2O5NiO as raw material, preparing 0.97 (Bi) according to stoichiometric ratio0.5Na0.5)TiO3-0.03Ba(Nb0.5Ni0.5)O3Ceramic powder. An organic monomer Acrylamide (AM) and a cross-linking agent N, N' -Methylene Bisacrylamide (MBAM) are weighed according to the mass ratio of 24:1, and are dissolved in deionized water according to the weight ratio to prepare a premixed liquid with the concentration of 5 wt.%. Preparing a ball milling tank, adding the prepared premixed liquid into the ball milling tank, weighing a certain amount of bismuth sodium titanate-based ceramic powder, and adding the bismuth sodium titanate-based ceramic powder (respectively adding 50 wt.%, 30 wt.%, and 20 wt.%) and a dispersant of polymethacrylic acid amine (PMAA-NH4) with corresponding mass into the premixed liquid for three times to obtain slurry with corresponding solid content. The solid content of the ceramic powder is kept at 45 vol.%, and the amount of the dispersing agent is 2 wt.% of the mass of the ceramic powder. Ball milling to obtain suspension solution with good flowability. Weighing a certain mass of ammonium persulfate solid, dissolving the ammonium persulfate solid in deionized water to prepare an initiator solution with the solution concentration of 2 wt.% for later use. The suspension solution in the ball mill pot was transferred to a beaker, and 5 wt.% of initiator solution and 2 wt.% of catalyst (N, N' -Tetramethylethylenediamine (TEMED)) were added based on the total mass of the organic monomer and the crosslinking agent, and magnetic stirring was performed under vacuum for 15 min. After the vacuum stirring is finished, the ceramic slurry is slowly injected into the mold along the mold wall, and the mold opening is sealed by a preservative film in time after the injection molding is finished, so that the pollution is prevented. The mold was allowed to stand at room temperature for 24h to ensure the slurry solidified. And (3) placing the solidified blank in a stable environment, adjusting the temperature to be 15 ℃ and the humidity to be 80%, drying for 4 days, adjusting the temperature to be 20 ℃ and the humidity to be 60%, and drying for 2 days until the quality of the blank is not changed, which indicates that the moisture in the blank is basically removed. Baking in 80 deg.C oven for 30min to completely dry. And (3) putting the dried blank into a muffle furnace, heating to 600 ℃ at the heating rate of 0.4 ℃/min, preserving the temperature for 2 hours, and cooling along with the furnace. And sintering the green body after the binder removal in a muffle furnace, wherein the sintering temperature is 1050 ℃, and the heat preservation time is 2 hours. The sodium bismuth titanate-based ferroelectric ceramic with compact structure and high strength can be prepared by gel casting technology.
Examples 2 to 4
The steps of example 2, example 3 and example 4 are the same as those of example 1, and the specific mixture ratio and the process parameters are different.
Wherein, the mixture ratio and the process parameters of the embodiment 1 to the embodiment 4 are shown in the table 1.
TABLE 1 examples 1-4 compounding ratios and Process tables
The performance of the sodium bismuth titanate-based ferroelectric ceramics obtained in examples 1 to 4 was analyzed to obtain the performance table of table 2, and it can be seen that the performance of the sodium bismuth titanate-based ferroelectric ceramics obtained in the above examples is better.
TABLE 2 Performance tables of Experimental results of examples 1 to 4
The bismuth sodium titanate-based ferroelectric ceramic is prepared by using a gel casting technology, ceramic powder, a dispersing agent, a solvent and other ingredients are mixed in a liquid state by adjusting a proper proportion and process parameters, and a blank body with a certain shape is obtained by removing the solvent and other methods, so that the agglomeration of particles can be effectively controlled, and a ceramic part with uniform components, good compactness, large size and complex shape is prepared. Compared with the traditional dry pressing, the agglomeration of ceramic particles can be effectively controlled by the gel injection molding technology, and the components are uniform in the ceramic forming process and the sintering process, so that the ceramic performance fluctuation caused by the nonuniform structure is avoided, and the stability and the reliability of the ceramic performance are improved.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A sodium bismuth titanate-based ferroelectric ceramic gel-casting preparation method is characterized by comprising the following steps:
preparing a premixed solution: weighing an organic monomer acrylamide and a cross-linking agent N, N '-methylene bisacrylamide according to a mass ratio of 12: 1-24: 1, and dissolving the organic monomer acrylamide and the cross-linking agent N, N' -methylene bisacrylamide in water to obtain a premixed solution with a concentration of 5-20 wt.%;
preparation of suspension solutions: adding sodium bismuth titanate-based ceramic powder and a dispersing agent into the premixed liquid, wherein the mass of the dispersing agent is 1-8 wt% of that of the ceramic powder, and the solid content of the ceramic powder is controlled to be 40-60 vol%;
initiator and catalyst addition: adding an initiator solution with the concentration of 1-8% of a catalyst and the solution into the suspension solution and stirring to obtain ceramic slurry, wherein the mass ratio of the initiator to the premixed solution is 5-30 wt%, and the mass ratio of the catalyst to the premixed solution is 1-10 wt%;
and (3) injection molding and curing: injecting the ceramic slurry into a mold for curing to obtain a ceramic blank;
drying the blank: drying the ceramic blank body in an environment with the temperature of 15-20 ℃ and the humidity of 80-90%;
and (3) blank glue discharging: regulating the heating rate to be 0.3-0.5 ℃/min, heating to 600 ℃, preserving the heat for 1-2 h, and cooling;
and (3) sintering of ceramics: the sintering temperature is 1030-1080 ℃, and the heat preservation time is 2-3 h.
2. The gel injection molding method for preparing a sodium bismuth titanate-based ferroelectric ceramic according to claim 1, wherein, in the preparation of the suspension solution, a ball milling tank is used as a container, and the premixed liquid, the sodium bismuth titanate-based ceramic powder and the dispersant are poured into the ball milling tank and ball milled to obtain the suspension solution.
3. The gel-casting method of preparing a sodium bismuth titanate-based ferroelectric ceramic according to claim 1, wherein the dispersant comprises polymethacrylic acid amine or citric acid amine.
4. The gel-casting method of a sodium bismuth titanate-based ferroelectric ceramic according to claim 1, wherein the initiator solution is an ammonium persulfate solution.
5. The gel injection molding method for preparing a sodium bismuth titanate-based ferroelectric ceramic according to claim 1, wherein the catalyst is N, N' -tetramethylethylenediamine.
6. The gel-casting preparation method of a sodium bismuth titanate-based ferroelectric ceramic according to claim 1, wherein the catalyst and the initiator solution having a solution concentration of 1% to 8% are added to the suspension solution and stirred, comprising,
and transferring the suspension solution into a beaker, adding the initiator solution and the catalyst, and carrying out magnetic stirring in a vacuum state to carry out vacuum defoaming for 10-50 min.
7. The gel-casting method of preparing a sodium bismuth titanate-based ferroelectric ceramic according to claim 1, wherein the mold is left at room temperature for 12 to 24 hours to solidify the ceramic slurry during the casting solidification.
8. The gel-casting method of preparing a sodium bismuth titanate-based ferroelectric ceramic according to claim 1, wherein the step of drying the green body comprises:
placing the ceramic blank in an environment with the temperature of 15-20 ℃ and the humidity of 80-90%, and drying for 3-5 days;
adjusting the humidity to 40% -60%, and drying for 1-2 days;
transferring the mixture to an oven with the temperature of 60-80 ℃ for baking for 30-60 min.
9. The gel-casting method of a sodium bismuth titanate-based ferroelectric ceramic according to claim 1, wherein the blank is placed in a muffle furnace for gel removal during gel removal.
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