CN113956618A - Preparation method of three-dimensional porous barium titanate composite dielectric material - Google Patents
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Abstract
The invention discloses a preparation method of a three-dimensional porous barium titanate composite dielectric material, and belongs to the technical field of dielectric material production. The preparation method of the three-dimensional porous barium titanate composite dielectric material comprises the following steps: firstly, the cotton felt is soaked in acetone solution for treatment and then soaked in TiCl4And BaCl2Putting the mixed solution into NaOH solution for reaction, and then sequentially carrying out aging, washing, ethanol soaking, drying and calcining to obtain a barium titanate three-dimensional porous material; and (3) adding a diluent and a curing agent into the epoxy resin, and adding the barium titanate three-dimensional porous material for curing to obtain the barium titanate three-dimensional porous material. The invention takes low-cost pure cotton felt as a framework, after barium titanate is adsorbed on the framework, the pure cotton felt is removed by calcination, then the pure cotton felt is cast by epoxy resin, and the three-dimensional porous barium titanate dielectric composite material is obtained after curing, wherein the durability of the three-dimensional porous structure is highGood dielectric property for long-term use, and the dielectric property is better than that of the composite material directly added with barium titanate.
Description
Technical Field
The invention belongs to the technical field of dielectric material production, and particularly relates to a preparation method of a three-dimensional porous barium titanate composite dielectric material.
Background
Barium titanate is an important material of a strong dielectric compound. Besides the characteristics of piezoelectricity, ferroelectricity, voltage resistance, excellent insulating property and the like, the composite material can be widely applied to the fields of functional ceramics, positive temperature coefficient thermistors, multilayer ceramic capacitors, biological medicines and the like. The ideal ceramic powder raw material needs to be of high purity, fine in particle size and in a dispersed state. The conventional methods for preparing barium titanate, such as a solid-phase synthesis method, a coprecipitation method, a sol-gel method, a hydrothermal synthesis method and the like, have the problems that the prepared products are seriously agglomerated and difficult to disperse, so that the dielectric property of barium titanate is greatly weakened.
In order to solve the problem of agglomeration of barium titanate, coupling agents and the like are commonly used to slow the agglomeration of barium titanate, but the barium titanate can not be well dispersed in use, and with the deep research, "preparation and application research of dendritic barium titanate powder" (Wangshiz, Beijing chemical university, chemical engineering and technology, 2018 Master thesis) proposes that certain distribution oriented barium titanate is provided, and the properties such as dielectric property, wave absorption and the like are excellent, so that a plurality of methods capable of distributing the barium titanate according to needs also appear at present. CN112280297A discloses a barium titanate/polyetherimide dielectric composite material and a preparation method thereof, which uses foamed nickel as a skeleton to prepare a barium titanate skeleton with a three-dimensional structure, but uses foamed nickel as the skeleton, and uses acid pickling to remove foamed nickel after the reaction is finished, so that the cost is high and certain environmental pollution is caused; CN112341190A discloses a method for preparing barium titanate-based powder, barium titanate-based powder and supercapacitor, wherein porous carbon is used as a template to prepare a dielectric material with controllable grain size and distribution, but porous carbon is used as a skeleton, which is high in cost and not beneficial to industrial production.
Disclosure of Invention
The invention provides a process method for preparing a three-dimensional porous barium titanate dielectric composite material, which comprises the steps of taking a low-cost cotton felt as a framework, removing the cotton felt through calcination after barium titanate is adsorbed on the framework, casting by using epoxy resin, and curing to obtain the three-dimensional porous barium titanate dielectric composite material.
The invention provides a preparation method of a three-dimensional porous barium titanate composite dielectric material, which comprises the following steps:
A. soaking the cotton felt in an acetone aqueous solution for treatment, and then washing and drying to obtain the treated cotton felt;
B. soaking the treated cotton felt obtained in the step A into TiCl4And BaCl2Taking out the mixed solution, then putting the mixed solution into NaOH solution for reaction, cooling the mixed solution to room temperature after the reaction is finished, aging the mixed solution, washing, soaking in ethanol, drying, and calcining the dried product to obtain a barium titanate three-dimensional porous material;
C. and (3) adding a diluent and a curing agent into the epoxy resin, uniformly mixing, casting the barium titanate three-dimensional porous material obtained in the step (B) until the barium titanate three-dimensional porous material is completely covered and is 0.2-1.0 mm higher, naturally curing at room temperature, and obtaining the three-dimensional porous barium titanate composite dielectric material after curing is completed.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step A, the thickness of the cotton felt is 0.5-3 mm.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step A, the volume ratio of acetone to water in the acetone aqueous solution is 10-20%.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step A, the treatment temperature is 40-70 ℃.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step A, the treatment time is 12-24 hours.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step A, the drying temperature is 70-90 ℃.
Wherein, the preparation method of the three-dimensional porous barium titanate composite dielectric material comprises the step B of TiCl4And BaCl2The mixed solution is prepared by the following method: mixing TiCl4Preparing an aqueous solution with a molar concentration of 0.2-1.0 mol/L, BaCl2Preparing an aqueous solution with a molar concentration of 0.2-1.0 mol/L, and then mixing the aqueous solution with a mixed solution of Ti and Ba according to a molar ratio of 1: 1.1 to 1.3 adding TiCl4Solution and BaCl2Mixing the solution, and adding TiCl in percentage by mass4Solution and BaCl2And (3) stirring the nonionic emulsifier OP-10 accounting for 0.1-0.5% of the total mass of the solution for 10-30 minutes at the rotating speed of 800-1200 rpm to obtain the aqueous emulsion.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step B, the molar concentration of the NaOH solution is 0.8-1.2 mol/L, and the temperature is 80-100 ℃.
In the step B, during the reaction in the NaOH solution, the rotating speed is controlled to be 500-1000 r/min, and the heat preservation reaction time is 1.5-3 hours.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step B, the aging time is 3-6 hours.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step B, the washing is distilled water washing for 3-5 times.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step B, the ethanol soaking is absolute ethanol soaking for 3-5 hours.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step B, the calcining temperature is 500-700 ℃.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step B, the calcining time is 1.5-3 hours.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step C, the diluent is propenyl glycidyl ether, butyl glycidyl ether or phenyl glycidyl ether.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step C, the addition amount of the diluent is 10-30% of the mass of the epoxy resin.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step C, the addition amount of the curing agent is calculated according to the epoxy group amount of the epoxy resin.
In the preparation method of the three-dimensional porous barium titanate composite dielectric material, in the step C, the curing time is 24-48 hours.
The invention has the beneficial effects that:
the invention takes the cheap pure cotton felt as the framework, after barium titanate is adsorbed on the framework, the pure cotton felt is removed by calcination, then the three-dimensional porous barium titanate dielectric composite material is obtained by casting and curing with the epoxy resin. The framework used in the invention is a natural porous material, the material is easy to obtain, the price is low, the preparation is simple, the three-dimensional porous structure has good durability, and the dielectric property can be supported to be good in long-term use; meanwhile, due to the introduction of a three-dimensional porous structure, the dielectric property of the composite material is better than that of a composite material directly added with barium titanate under the same addition of barium titanate.
Detailed Description
Specifically, the preparation method of the three-dimensional porous barium titanate composite dielectric material comprises the following steps:
A. soaking the cotton felt in an acetone aqueous solution for treatment, and then washing and drying to obtain the treated cotton felt;
B. soaking the treated cotton felt obtained in the step A into TiCl4And BaCl2Taking out the mixed solution, then putting the mixed solution into NaOH solution for reaction, cooling the mixed solution to room temperature after the reaction is finished, aging the mixed solution, washing, soaking in ethanol, drying, and calcining the dried product to obtain a barium titanate three-dimensional porous material;
C. and (3) adding a diluent and a curing agent into the epoxy resin, uniformly mixing, casting the barium titanate three-dimensional porous material obtained in the step (B) until the barium titanate three-dimensional porous material is completely covered and is 0.2-1.0 mm higher, naturally curing at room temperature, and obtaining the three-dimensional porous barium titanate composite dielectric material after curing is completed.
In the step A, the cotton felt with the corresponding thickness is taken according to the requirement, and the thickness is generally 0.5-3 mm.
In the step A, an acetone aqueous solution with the volume ratio of acetone to water of 10-20% is adopted, the cotton felt is placed into the acetone aqueous solution to be treated for 12-24 hours at the temperature of 40-70 ℃, and the cotton felt is dried at the temperature of 70-90 ℃ after being washed clean by distilled water.
If the barium titanate solution is directly used, the barium titanate solution is not easy to adhere to the cotton felt, so the TiCl is used in the invention4And BaCl2Mixed liquid, which can make the inside of the cotton felt also have TiCl4And BaCl2The mixed liquid has more attachment amount and better attachment effect. The TiCl4And BaCl2The mixed solution is prepared by the following method: mixing TiCl4Preparing an aqueous solution with a molar concentration of 0.2-1.0 mol/L, BaCl2Preparing an aqueous solution with a molar concentration of 0.2-1.0 mol/L, and then mixing the aqueous solution with a mixed solution of Ti and Ba according to a molar ratio of 1: 1.1 to 1.3 adding TiCl4Solution and BaCl2Mixing the solution, and adding TiCl in percentage by mass4Solution and BaCl2And (3) stirring the nonionic emulsifier OP-10 accounting for 0.1-0.5% of the total mass of the solution for 10-30 minutes at the rotating speed of 800-1200 rpm to obtain the aqueous emulsion.
In the step B, NaOH solution with the molar concentration of 0.8-1.2 mol/L is used as a mineralizer, the mineralizer is heated to 80-100 ℃, the rotating speed is controlled to be 500-1000 r/min under the concentration range and high temperature, the heat preservation reaction time is 1.5-3 hours, and barium titanate is promoted to be generated.
In the step B, after the reaction is finished, the aging time is 3-6 hours, then the mixture is washed by distilled water for 3-5 times, soaked by absolute ethyl alcohol for 3-5 hours, and calcined at 500-700 ℃ for 1.5-3 hours to obtain the barium titanate three-dimensional porous material.
In step C of the present invention, a reactive diluent commonly used in the art, such as propenyl glycidyl ether, butyl glycidyl ether or phenyl glycidyl ether; the addition amount of the diluent is controlled to be 10-30% of the mass of the epoxy resin, and the viscosity of the epoxy resin is reduced, so that subsequent smooth casting and forming can be realized. The invention can adopt various grades of epoxy resins sold on the market, and the addition amount of the curing agent can be calculated according to the epoxy group amount of the epoxy resin and the conventional addition amount in the field because the epoxy group amounts of different grades of the epoxy resins sold on the market are different. The curing agent of the present invention is a conventional ordinary-temperature curing agent in the art, and is applicable to aliphatic polyamine (diethylenetriamine), alicyclic polyamine, low-molecular polyamide, modified aromatic amine, and the like.
In the step C of the invention, the curing time is 24-48 hours.
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Pretreatment of the pure cotton felt: taking a pure cotton felt with the thickness of 1.5mm, and soaking the pure cotton felt in a mixture of acetone and water in a volume ratio of 1: 5 at 50 deg.C for 12 hr, washing with distilled water, and oven drying at 80 deg.C.
Epoxy resin (815), with an epoxy value of 180-190, was purchased from Wuxi Renzue chemical products, Inc.
Epoxy resin dilution: adding a diluent (501, namely butyl glycidyl ether) and a diethylenetriamine curing agent (the mass ratio of the diethylenetriamine curing agent to the epoxy resin 815 is 1: 9) into the epoxy resin in a mass percentage of 10-30% of the mass of the epoxy resin, and uniformly mixing to obtain the diluted epoxy resin.
Example 1
TiCl4And BaCl2Preparing a mixed solution: adding TiCl with a molar concentration of 0.2mol/L4An aqueous solution and BaCl with a molar concentration of 0.2mol/L2An aqueous solution, in a molar ratio of Ti/Ba of 1: 1.1 mixing and adding TiCl4Aqueous solution and BaCl2OP-10 with the total mass of 0.1 percent of the aqueous solution and the rotating speed of 800 revolutions per minute is stirred for 30 minutes to obtain TiCl4And BaCl2And (4) mixing the solution.
Soaking the treated cotton felt into TiCl at room temperature4And BaCl2Immediately taking out the mixed solution, putting the mixed solution into NaOH solution with the molar concentration of 0.8mol/L and the temperature of 100 ℃, reacting for 1.5 hours at the rotating speed of 500 revolutions per minute, cooling to room temperature, aging for 3 hours, washing with distilled water for 3 times, soaking in absolute ethyl alcohol for 3 hours, drying, putting into a muffle furnace, and calcining for 3 hours at the temperature of 500 ℃ to obtain the barium titanate three-dimensional porous material; slowly pouring the epoxy resin diluted and added with the curing agent into the barium titanateThe three-dimensional porous material is completely immersed and is higher than 0.3mm, the curing is carried out for 24 hours at room temperature, the prepared product is tested in the same way as the barium titanate/epoxy resin composite material with the same addition amount of barium titanate and the same thickness, the breakdown strength is improved by 7.2 percent, and the dielectric constant is improved by 5.4 percent.
Example 2
TiCl4And BaCl2Preparing a mixed solution: TiCl with a molar concentration of 0.6mol/L4An aqueous solution and BaCl with a molar concentration of 0.6mol/L2An aqueous solution, in a molar ratio of Ti/Ba of 1: 1.2 mixing and adding TiCl4Aqueous solution and BaCl2OP-10 with the total mass of 0.3 percent of the aqueous solution and the rotating speed of 1000 revolutions per minute is stirred for 20 minutes to obtain TiCl4And BaCl2And (4) mixing the solution.
Soaking the treated cotton felt into TiCl at room temperature4And BaCl2Immediately taking out the mixed solution, putting the mixed solution into a NaOH solution with the molar concentration of 1.0mol/L and the temperature of 90 ℃, reacting for 2.5 hours at the rotating speed of 700 revolutions per minute, cooling to room temperature, aging for 4 hours, washing with distilled water for 4 times, soaking in absolute ethyl alcohol for 4 hours, drying, putting the mixture into a muffle furnace, and calcining for 2 hours at the temperature of 600 ℃ to obtain the barium titanate three-dimensional porous material; and slowly pouring the epoxy resin diluted and added with the curing agent into the barium titanate three-dimensional porous material, completely immersing the barium titanate three-dimensional porous material by 0.6mm, curing the barium titanate three-dimensional porous material at room temperature for 32 hours, and performing the same test on the prepared product and the barium titanate/epoxy resin composite material with the same barium titanate adding amount and the same thickness, wherein the breakdown strength is improved by 6.3 percent, and the dielectric constant is improved by 4.3 percent.
Example 3
TiCl4And BaCl2Preparing a mixed solution: adding TiCl with a molar concentration of 1.0mol/L4An aqueous solution and BaCl with a molar concentration of 1.0mol/L2An aqueous solution, in a molar ratio of Ti/Ba of 1: 1.3 mixing and adding TiCl4Aqueous solution and BaCl2OP-10 with the total mass of 0.5 percent of the aqueous solution and the rotating speed of 1200 r/min is stirred for 10 min to obtain TiCl4And BaCl2And (4) mixing the solution.
Soaking the treated cotton felt into TiCl at room temperature4And BaCl2Immediately taking out the mixed solution, putting the mixed solution into a NaOH solution with the molar concentration of 1.2mol/L and the temperature of 80 ℃, reacting for 3 hours at the rotating speed of 1000 revolutions per minute, cooling to room temperature, aging for 6 hours, washing with distilled water for 5 times, soaking in absolute ethyl alcohol for 5 hours, drying, putting into a muffle furnace, and calcining for 1.5 hours at the temperature of 700 ℃ to obtain a barium titanate three-dimensional porous material; and slowly pouring the epoxy resin diluted and added with the curing agent into the barium titanate three-dimensional porous material, completely immersing the barium titanate three-dimensional porous material by 0.9mm, curing the barium titanate three-dimensional porous material at room temperature for 48 hours, and performing the same test on the prepared product and the barium titanate/epoxy resin composite material with the same barium titanate adding amount and the same thickness, wherein the breakdown strength is improved by 6.8 percent, and the dielectric constant is improved by 4.8 percent.
Claims (10)
1. The preparation method of the three-dimensional porous barium titanate composite dielectric material is characterized by comprising the following steps: the method comprises the following steps:
A. soaking the cotton felt in an acetone aqueous solution for treatment, and then washing and drying to obtain the treated cotton felt;
B. soaking the treated cotton felt obtained in the step A into TiCl4And BaCl2Taking out the mixed solution, then putting the mixed solution into NaOH solution for reaction, cooling the mixed solution to room temperature after the reaction is finished, aging the mixed solution, washing, soaking in ethanol, drying, and calcining the dried product to obtain a barium titanate three-dimensional porous material;
C. and (3) adding a diluent and a curing agent into the epoxy resin, uniformly mixing, casting the barium titanate three-dimensional porous material obtained in the step (B) until the barium titanate three-dimensional porous material is completely covered and is 0.2-1.0 mm higher, naturally curing at room temperature, and obtaining the three-dimensional porous barium titanate composite dielectric material after curing is completed.
2. The method for preparing a three-dimensional porous barium titanate composite dielectric material according to claim 1, wherein: in the step A, the thickness of the cotton felt is 0.5-3 mm.
3. The method for preparing a three-dimensional porous barium titanate composite dielectric material according to claim 1, wherein: in the step A, at least one of the following items is satisfied:
the volume ratio of acetone to water in the acetone aqueous solution is 10-20%;
the treatment temperature is 40-70 ℃;
the treatment time is 12-24 hours;
the drying temperature is 70-90 ℃.
4. The method for preparing a three-dimensional porous barium titanate composite dielectric material according to claim 1, wherein: in step B, the TiCl4And BaCl2The mixed solution is prepared by the following method: mixing TiCl4Preparing an aqueous solution with a molar concentration of 0.2-1.0 mol/L, BaCl2Preparing an aqueous solution with a molar concentration of 0.2-1.0 mol/L, and then mixing the aqueous solution with a mixed solution of Ti and Ba according to a molar ratio of 1: 1.1 to 1.3 adding TiCl4Solution and BaCl2Mixing the solution, and adding TiCl in percentage by mass4Solution and BaCl2And (3) stirring the nonionic emulsifier OP-10 accounting for 0.1-0.5% of the total mass of the solution for 10-30 minutes at the rotating speed of 800-1200 rpm to obtain the aqueous emulsion.
5. The method for preparing a three-dimensional porous barium titanate composite dielectric material according to claim 1, wherein: in the step B, the molar concentration of the NaOH solution is 0.8-1.2 mol/L, and the temperature is 80-100 ℃.
6. The method for preparing a three-dimensional porous barium titanate composite dielectric material according to claim 1, wherein: in the step B, when the reaction is carried out in the NaOH solution, the rotating speed is controlled to be 500-1000 r/min, and the heat preservation reaction time is 1.5-3 hours.
7. The method for preparing a three-dimensional porous barium titanate composite dielectric material according to claim 1, wherein: in the step B, at least one of the following items is satisfied:
the aging time is 3-6 hours;
the washing is distilled water washing for 3-5 times;
the ethanol soaking is absolute ethanol soaking for 3-5 hours;
the calcining temperature is 500-700 ℃;
the calcining time is 1.5-3 hours.
8. The method for preparing a three-dimensional porous barium titanate composite dielectric material according to claim 1, wherein: in the step C, the diluent is propenyl glycidyl ether, butyl glycidyl ether or phenyl glycidyl ether; the addition amount of the diluent is 10-30% of the mass of the epoxy resin.
9. The method for preparing a three-dimensional porous barium titanate composite dielectric material according to claim 1, wherein: in the step C, the addition amount of the curing agent is calculated according to the epoxy group amount of the epoxy resin.
10. The method for preparing the three-dimensional porous barium titanate composite dielectric material according to any one of claims 1 to 9, wherein: in the step C, the curing time is 24-48 hours.
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| CN112280297A (en) * | 2020-10-26 | 2021-01-29 | 中国海洋大学 | Barium titanate/polyetherimide dielectric composite material and preparation method thereof |
| CN112341190A (en) * | 2019-08-06 | 2021-02-09 | 广州汽车集团股份有限公司 | Barium titanate-based powder preparation method, barium titanate-based powder and supercapacitor |
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| WO1992018213A1 (en) * | 1991-04-12 | 1992-10-29 | E.I. Du Pont De Nemours And Company | High dielectric constant flexible ceramic composite |
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