CN114315349A - Method for preparing mesoporous barium zirconate titanate ceramic nanoparticles - Google Patents
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Abstract
The invention discloses a method for preparing mesoporous barium zirconate titanate ceramic nanoparticles, belonging to the technical field of electronic ceramic materials. The method adopts barium chloride (BaCl)2) As the barium salt, zirconium oxychloride (ZrOCl)2) As zirconium source, butyl titanate (C)16H36O4Ti) as a titanium source, ethylene glycol (C)2H6O2) As a reaction chelating agent, the mesoporous barium zirconate titanate nano material is successfully prepared by controlling the crystal growth speed through the rotary evaporation reaction under the high-concentration alkaline condition. The method mainly uses common inorganic salt and simple reagents in the synthesis process, has low cost, is simple and feasible, has good repeatability, is suitable for large-scale production, and can promote the commercialization process of electronic ceramic materials.
Description
Technical Field
The invention belongs to the technical field of electronic ceramic materials, and particularly relates to a method for preparing mesoporous barium zirconate titanate ceramic nanoparticles, namely a method for preparing a barium zirconate titanate nano material by using a rotary evaporation method.
Background
With the continuous progress of scientific technology and the rapid development of the microelectronics industry, higher requirements and challenges are put on the manufacture and use of electronic devices. Ceramic capacitors have an important position in microelectronic devices due to their advantages of high temperature resistance, corrosion resistance, high dielectric constant, and the like.
Barium titanate-based ceramics are known as the backbone of the electronics industry, and researchers have applied them over a wider temperature range by doping and modifying them. Barium titanate-based materials are widely used in various fields of ferroelectric, piezoelectric, and dielectric materials. With the rapid development of electronic components toward high precision, multifunction and miniaturization, higher requirements are placed on the purity, particle size and molding characteristics of ceramic powder. The barium strontium titanate ceramic is easy to break down under the action of an external direct current electric field, and is not beneficial to miniaturization of devices, so that the application of the barium strontium titanate ceramic is limited. Zr4+Is greater than Ti4+Has a larger ionic radius, so Zr4+Substituted Ti4+The chemical structure of the product is more stable. The barium titanate ceramic is in a tetragonal phase structure at normal temperature, and the Barium Zirconate Titanate (BZT) is formed by doping Zr in the barium titanate, so that the crystal structure can be greatly improved, and the room-temperature dielectric coefficient of the material can be greatly regulated.
The invention adopts barium chloride (BaCl)2) As the barium salt, zirconium oxychloride (ZrOCl)2) As zirconium source, butyl titanate (C)16H36O4Ti) as a titanium source, ethylene glycol (C)2H6O2) As a reaction chelating agent, the mesoporous barium zirconate titanate nano material is successfully prepared by controlling the crystal growth speed through the rotary evaporation reaction under the high-concentration alkaline condition. The method has the advantages of simple and feasible synthesis process, low synthesis temperature, good repeatability, high purity of the synthesized product, wide application prospect and the like, and can be used for ceramic capacitors and the like.
Disclosure of Invention
The invention aims to provide a method for preparing mesoporous barium zirconate titanate ceramic nano particles, and researches a barium zirconate titanate ceramic powder which is simple in preparation process, low in cost, non-toxic and harmless in product, high in purity, superfine and uniform and controllable in components.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing mesoporous barium zirconate titanate ceramic nanoparticles comprises the following steps:
step 1, preparing an ethylene glycol solution: weighing 0.776-3.104g C2H6O2Adding 20mL of deionized water into a beaker, and stirring until the deionized water is completely dissolved to obtain an ethylene glycol solution;
step 2, preparing a mixed solution: weighing 6.137-24.549g BaCl2Adding 20-80mL of deionized water into a beaker, stirring until the deionized water is completely dissolved, and weighing 4.279-17.114g of ZrOCl2Stirring until the mixture is completely dissolved to obtain a mixed solution;
step 3, preparing a titanium salt solution: weighing 4.25-17mL of C16H36O4Adding 10mL of absolute ethyl alcohol into the Ti in a beaker, and fully and uniformly stirring to obtain a titanium salt solution;
step 4, preparing an alkaline solution: weighing 12.5-50g of NaOH powder, adding a small amount of the weighed NaOH powder into 20-80mL of deionized water for multiple times, and uniformly stirring to obtain an alkaline solution;
step 5, preparing a precursor solution: sequentially adding the mixed solution obtained in the step 2, the titanium salt solution obtained in the step 3 and the alkaline solution obtained in the step 4 into the ethylene glycol solution obtained in the step 1, and continuously stirring to obtain a white turbid solution, namely a barium zirconate titanate precursor solution;
step 6, preparing precursor powder by rotary evaporation: transferring the barium zirconate titanate precursor solution obtained in the step (5) into an eggplant-shaped bottle, performing rotary evaporation reaction, centrifugally washing, and drying in an oven to obtain barium zirconate titanate precursor powder;
and 7, preparing a barium zirconate titanate nano material by high-temperature sintering: and (4) placing the barium zirconate titanate precursor powder obtained in the step (6) in a muffle furnace, and calcining at high temperature in the air to obtain the mesoporous barium zirconate titanate nano-particles.
In the technical scheme, the stirring process in the steps 1, 2, 3, 4 and 5 is carried out by using a magnetic stirrer, and the stirring time is 10-60 min.
In the above technical scheme, the process of adding the NaOH powder into the deionized water in the step 4 is divided into 5-10 times.
In the above technical solution, the conditions of the rotary evaporation in step 6 are as follows: rotationally steaming at 142MPa and 55 ℃ for 30-60min, and then rotationally steaming at 72MPa and 60 ℃ for 60-120 min; during centrifugal washing, firstly washing with ultrapure water for 3 times, and then washing with absolute ethyl alcohol for 3 times; finally, drying the barium zirconate titanate precursor powder in a drying oven at the temperature of 60 ℃ for 24-48h to obtain barium zirconate titanate precursor powder;
in the technical scheme, the calcination temperature in the step 7 is 800 ℃, and the heat preservation time is 120 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for preparing mesoporous barium zirconate titanate ceramic nano particles, which adopts barium chloride (BaCl)2) As the barium salt, zirconium oxychloride (ZrOCl)2) As zirconium source, butyl titanate (C)16H36O4Ti) as a titanium source, ethylene glycol (C)2H6O2) As a reaction chelating agent, the mesoporous barium zirconate titanate nano material is successfully prepared by controlling the crystal growth speed through the rotary evaporation reaction under the high-concentration alkaline condition. The method is low in cost, simple and easy to implement, good in repeatability, suitable for large-scale production and capable of promoting the commercialization process of the electronic ceramic material.
Drawings
FIG. 1 is a flow chart of a process for preparing mesoporous barium zirconate titanate ceramic nanoparticles according to the present invention;
FIG. 2 is an X-ray diffraction pattern of the mesoporous barium zirconate titanate nano-material prepared in example 3 of the present invention;
FIG. 3 is a scanning electron microscope image of the mesoporous barium zirconate titanate nano-material prepared in example 3 of the present invention;
fig. 4 is a transmission electron microscope image of the mesoporous barium zirconate titanate nano-material prepared in example 3 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: a method for preparing mesoporous barium zirconate titanate ceramic nanoparticles is shown in a process flow chart of figure 1, and comprises the following specific operation steps:
step 1, preparing an ethylene glycol solution: weighing 0.776-3.104g C2H6O2Adding 20mL of deionized water into a beaker, and stirring for 10min by using a magnetic stirrer to obtain an ethylene glycol solution;
step 2, preparing a mixed solution: weighing 6.137-24.549g BaCl2Adding 20-80mL deionized water into a beaker, stirring for 10-30min by using a magnetic stirrer, and weighing 4.279-17.114g ZrOCl2Stirring for 10-30min by using a magnetic stirrer to obtain a mixed solution;
step 3, preparing a titanium salt solution: weighing 4.25-17mL of C16H36O4Adding 10mL of absolute ethyl alcohol into the Ti in a beaker, and stirring for 10-30min by using a magnetic stirrer to obtain a titanium salt solution;
step 4, preparing an alkaline solution: weighing 12.5-50g of NaOH powder, adding the weighed NaOH powder into 20-80mL of deionized water for 5-10 times, and stirring for 10-30min by using a magnetic stirrer to obtain an alkaline solution;
step 5, preparing a precursor solution: sequentially adding the mixed solution obtained in the step 2, the titanium salt solution obtained in the step 3 and the alkaline solution obtained in the step 4 into the ethylene glycol solution obtained in the step 1, and stirring for 30-60min by using a magnetic stirrer to obtain a barium zirconate titanate precursor solution;
step 6, preparing precursor powder by rotary evaporation: transferring the barium zirconate titanate precursor solution obtained in the step (5) into an eggplant-shaped bottle, and performing rotary evaporation at 142MPa and 55 ℃ for 30-60min, and then performing rotary evaporation at 72MPa and 60 ℃ for 60-120 min; during centrifugal washing, firstly washing with ultrapure water for 3 times, and then washing with absolute ethyl alcohol for 3 times; finally, drying the mixture in an oven at 60 ℃ for 24-48h to obtain barium zirconate titanate precursor powder;
and 7, preparing a barium zirconate titanate nano material by high-temperature sintering: and (3) placing the barium zirconate titanate precursor powder obtained in the step (6) in a muffle furnace, and calcining at high temperature in the air, wherein the calcining temperature is 800 ℃, and the heat preservation time is 120min, so that the mesoporous barium zirconate titanate nano-particles can be obtained.
Example 1:
step 1, preparing an ethylene glycol solution: weigh 0.776g C2H6O2Adding 20mL of deionized water into a beaker, and stirring for 10min by using a magnetic stirrer to obtain an ethylene glycol solution;
step 2, preparing a mixed solution: 6.137g of BaCl were weighed out2Adding 20mL of deionized water into a beaker, stirring for 10min by using a magnetic stirrer, and weighing 4.279g of ZrOCl2Stirring for 10min by using a magnetic stirrer to obtain a mixed solution;
step 3, preparing a titanium salt solution: the amount of C was measured to be 4.25mL16H36O4Adding 10mL of absolute ethyl alcohol into the Ti in a beaker, and stirring for 10min by using a magnetic stirrer to obtain a titanium salt solution;
step 4, preparing an alkaline solution: weighing 12.5g of NaOH powder, adding the weighed NaOH powder into 20mL of deionized water for 5 times, and stirring for 10min by using a magnetic stirrer to obtain an alkaline solution;
step 5, preparing a precursor solution: sequentially adding the mixed solution obtained in the step 2, the titanium salt solution obtained in the step 3 and the alkaline solution obtained in the step 4 into the ethylene glycol solution obtained in the step 1, and stirring for 30min by using a magnetic stirrer to obtain a barium zirconate titanate precursor solution;
step 6, preparing precursor powder by rotary evaporation: transferring the barium zirconate titanate precursor solution obtained in the step (5) into an eggplant-shaped bottle, and performing rotary evaporation at 142MPa and 55 ℃ for 30min and then performing rotary evaporation at 72MPa and 60 ℃ for 60 min; during centrifugal washing, firstly washing with ultrapure water for 3 times, and then washing with absolute ethyl alcohol for 3 times; finally, drying the barium zirconate titanate precursor powder in a drying oven at 60 ℃ for 24 hours to obtain barium zirconate titanate precursor powder;
and 7, preparing a barium zirconate titanate nano material by high-temperature sintering: and (3) placing the barium zirconate titanate precursor powder obtained in the step (6) in a muffle furnace, and calcining at high temperature in the air, wherein the calcining temperature is 800 ℃, and the heat preservation time is 120min, so that the mesoporous barium zirconate titanate nano-particles can be obtained.
Example 2:
step 1, preparing an ethylene glycol solution: weigh 1.552g C2H6O2Adding 20mL of deionized water into a beaker, and stirring for 10min by using a magnetic stirrer to obtain an ethylene glycol solution;
step 2, preparing a mixed solution: 12.275g of BaCl were weighed out2Adding 40mL of deionized water into a beaker, stirring for 20min by using a magnetic stirrer, and weighing 8.557g of ZrOCl2Stirring for 20min by using a magnetic stirrer to obtain a mixed solution;
step 3, preparing a titanium salt solution: the amount of C was measured to be 8.5mL16H36O4Adding 10mL of absolute ethyl alcohol into the Ti in a beaker, and stirring for 20min by using a magnetic stirrer to obtain a titanium salt solution;
step 4, preparing an alkaline solution: weighing 25g of NaOH powder, adding the weighed NaOH powder into 40mL of deionized water for 8 times, and stirring for 20min by using a magnetic stirrer to obtain an alkaline solution;
step 5, preparing a precursor solution: sequentially adding the mixed solution obtained in the step 2, the titanium salt solution obtained in the step 3 and the alkaline solution obtained in the step 4 into the ethylene glycol solution obtained in the step 1, and stirring for 45min by using a magnetic stirrer to obtain a barium zirconate titanate precursor solution;
step 6, preparing precursor powder by rotary evaporation: transferring the barium zirconate titanate precursor solution obtained in the step (5) into an eggplant-shaped bottle, and performing rotary evaporation at 142MPa and 55 ℃ for 45min and then performing rotary evaporation at 72MPa and 60 ℃ for 90 min; during centrifugal washing, firstly washing with ultrapure water for 3 times, and then washing with absolute ethyl alcohol for 3 times; finally, drying the barium zirconate titanate powder in a drying oven at 60 ℃ for 30 hours to obtain barium zirconate titanate precursor powder;
and 7, preparing a barium zirconate titanate nano material by high-temperature sintering: and (3) placing the barium zirconate titanate precursor powder obtained in the step (6) in a muffle furnace, and calcining at high temperature in the air, wherein the calcining temperature is 800 ℃, and the heat preservation time is 120min, so that the mesoporous barium zirconate titanate nano-particles can be obtained.
Example 3:
step 1, preparing an ethylene glycol solution: weighing 3.104g C2H6O2Adding 20mL of deionized water into a beaker, and stirring for 10min by using a magnetic stirrer to obtain an ethylene glycol solution;
step 2, preparing a mixed solution: 24.549g of BaCl were weighed out2Adding 80mL of deionized water into a beaker, stirring for 30min by using a magnetic stirrer, and weighing 17.114g of ZrOCl2Stirring for 30min by using a magnetic stirrer to obtain a mixed solution;
step 3, preparing a titanium salt solution: weighing 17mL of C16H36O4Adding 10mL of absolute ethyl alcohol into the Ti in a beaker, and stirring for 30min by using a magnetic stirrer to obtain a titanium salt solution;
step 4, preparing an alkaline solution: weighing 50g of NaOH powder, adding the weighed NaOH powder into 80mL of deionized water by 10 times, and stirring for 30min by using a magnetic stirrer to obtain an alkaline solution;
step 5, preparing a precursor solution: sequentially adding the mixed solution obtained in the step 2, the titanium salt solution obtained in the step 3 and the alkaline solution obtained in the step 4 into the ethylene glycol solution obtained in the step 1, and stirring for 60min by using a magnetic stirrer to obtain a barium zirconate titanate precursor solution;
step 6, preparing precursor powder by rotary evaporation: transferring the barium zirconate titanate precursor solution obtained in the step (5) into an eggplant-shaped bottle, and performing rotary evaporation at 142MPa and 55 ℃ for 60min and then performing rotary evaporation at 72MPa and 60 ℃ for 120 min; during centrifugal washing, firstly washing with ultrapure water for 3 times, and then washing with absolute ethyl alcohol for 3 times; finally, drying the barium zirconate titanate powder in a drying oven at the temperature of 60 ℃ for 48 hours to obtain barium zirconate titanate precursor powder;
and 7, preparing a barium zirconate titanate nano material by high-temperature sintering: and (3) placing the barium zirconate titanate precursor powder obtained in the step (6) in a muffle furnace, and calcining at high temperature in the air, wherein the calcining temperature is 800 ℃, and the heat preservation time is 120min, so that the mesoporous barium zirconate titanate nano material can be obtained.
The barium zirconate titanate nano-material prepared in the embodiment 3 of the invention is subjected to X-ray diffraction analysis (XRD) (as shown in figure 2), and the characteristic peak of barium zirconate titanate in the nano-material is shown and corresponds to the standard card, and the bifurcation in the diffraction peak is caused by the formation of the barium zirconate titanate solid solution. The prepared barium zirconate titanate nano material has good crystallinity and basically has no impurity phase. Therefore, the conclusion that the barium zirconate titanate nano material is successfully prepared by the method can be drawn.
The morphology of the barium zirconate titanate nano material prepared in the embodiment 3 of the present invention is analyzed by using a Scanning Electron Microscope (SEM) (as shown in fig. 3), and it can be seen that the barium zirconate titanate nano particles are uniformly distributed, and the average particle size is 45nm, which proves that the high-purity ultrafine barium zirconate titanate nano material with uniformly controllable components can be successfully prepared by using the method of the present invention.
The morphology and structure of the barium zirconate titanate nano material prepared in embodiment 3 of the present invention are analyzed by a transmission electron microscope (SEM) (as shown in fig. 4), it can be seen that the barium zirconate titanate nano particles have a uniform size distribution and a pore diameter of about 7nm, which belongs to a mesoporous scale, and it is proved that the method of the present invention can successfully prepare a high-purity ultrafine mesoporous barium zirconate titanate nano material with uniform and controllable components.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for preparing mesoporous barium zirconate titanate ceramic nanoparticles is characterized by comprising the following steps:
step 1, preparing an ethylene glycol solution: weighing 0.776-3.104g C2H6O2Adding 20mL of deionized water into a beaker, and stirring until the deionized water is completely dissolved to obtain an ethylene glycol solution;
step 2, preparing a mixed solution: 6.137-24 were weighed.549g BaCl2Adding 20-80mL of deionized water into a beaker, stirring until the deionized water is completely dissolved, and weighing 4.279-17.114g of ZrOCl2Stirring until the mixture is completely dissolved to obtain a mixed solution;
step 3, preparing a titanium salt solution: weighing 4.25-17mL of C16H36O4Adding 10mL of absolute ethyl alcohol into the Ti in a beaker, and fully and uniformly stirring to obtain a titanium salt solution;
step 4, preparing an alkaline solution: weighing 12.5-50g of NaOH powder, adding a small amount of the weighed NaOH powder into 20-80mL of deionized water for multiple times, and uniformly stirring to obtain an alkaline solution;
step 5, preparing a precursor solution: sequentially adding the mixed solution obtained in the step 2, the titanium salt solution obtained in the step 3 and the alkaline solution obtained in the step 4 into the ethylene glycol solution obtained in the step 1, and continuously stirring to obtain a white turbid solution, namely a barium zirconate titanate precursor solution;
step 6, preparing precursor powder by rotary evaporation: transferring the barium zirconate titanate precursor solution obtained in the step (5) into an eggplant-shaped bottle, performing rotary evaporation reaction, centrifugally washing, and drying in an oven to obtain barium zirconate titanate precursor powder;
and 7, preparing a barium zirconate titanate nano material by high-temperature sintering: and (4) placing the barium zirconate titanate precursor powder obtained in the step (6) in a muffle furnace, and calcining at high temperature in the air to obtain the mesoporous barium zirconate titanate nano-particles.
2. The method for preparing mesoporous barium zirconate titanate ceramic nanoparticles according to claim 1, wherein the stirring process in steps 1, 2, 3, 4 and 5 is performed by using a magnetic stirrer, and the stirring time is 10-60 min.
3. The method for preparing mesoporous barium zirconate titanate ceramic nanoparticles according to claim 1, wherein the step 4 is carried out by adding 5-10 times of NaOH powder into deionized water.
4. The method for preparing mesoporous barium zirconate titanate ceramic nanoparticles according to claim 1, wherein the conditions of the rotary evaporation in the step 6 are as follows: rotationally steaming at 142MPa and 55 ℃ for 30-60min, and then rotationally steaming at 72MPa and 60 ℃ for 60-120 min; during centrifugal washing, firstly washing with ultrapure water for 3 times, and then washing with absolute ethyl alcohol for 3 times; finally, drying the barium zirconate titanate precursor powder in an oven at the temperature of 60 ℃ for 24 to 48 hours to obtain the barium zirconate titanate precursor powder.
5. The method for preparing mesoporous barium zirconate titanate ceramic nanoparticles according to claim 1, wherein the calcination temperature in step 7 is 800 ℃ and the holding time is 120 min.
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