CN110171966B - Preparation method of barium titanate-artificially synthesized fluorophlogopite composite material - Google Patents

Preparation method of barium titanate-artificially synthesized fluorophlogopite composite material Download PDF

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CN110171966B
CN110171966B CN201910464922.0A CN201910464922A CN110171966B CN 110171966 B CN110171966 B CN 110171966B CN 201910464922 A CN201910464922 A CN 201910464922A CN 110171966 B CN110171966 B CN 110171966B
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barium titanate
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李祈霖
黄腾
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Meizhou Sanbao Guangguang Mica Technology Co ltd
Guangdong Triratna New Material Science And Technology Co ltd
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Meizhou Sanbao Guangguang Mica Technology Co ltd
Guangdong Triratna New Material Science And Technology Co ltd
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    • C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
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Abstract

A barium titanate-artificially synthesized fluorophlogopite composite material is prepared through liquid-phase deposition of TiCl4、BaCl2Gradually dropping NaOH into a reaction kettle filled with synthetic mica powder, and reacting to form nano-scale BaTiO under the conditions of certain temperature and pH value3Depositing on the surface of the synthetic mica powder, dehydrating and washing to finally obtain the barium titanate-artificially synthesized fluorophlogopite composite material. The barium titanate-artificially synthesized fluorophlogopite composite material improves the purity and the particle size controllability of barium titanate, reduces the use cost of the barium titanate material, and meets the market demand on the high-purity barium titanate material.

Description

Preparation method of barium titanate-artificially synthesized fluorophlogopite composite material
Technical Field
The invention relates to the field of research and development of composite materials, in particular to a preparation method of a barium titanate-artificially synthesized fluorophlogopite composite material.
Background
Perovskites (perovskites) are minerals named under the name of russian geologist Perovski. The composition of perovskite in the narrow sense is limited to CaTiO3Whereas perovskite in the broadest sense means ABX of the type having a perovskite structure3A compound of the formula (I). BX with perovskite structure connected by three-dimensional space corner-sharing top6Octahedral composition, wherein A is a large radius cation (e.g. Na)+、K+、Ca2+、Sr2+、Pb2+、Ba2+Etc.), B is a small radius cation (e.g., Ti)4+、Nb5+、Mn4+、Fe3+、Ni3+、Ta5+Etc.), X is an anion (O)2-、F-、Br-Etc.). Since different kinds and different amounts of elements can be accommodated at the A, B and X sites, compounds having perovskite-type structures are very bulky and they have found extremely wide application in fields such as geology, material science, and the like. For example, the most predominant mineral phase of the lower mantle, MgSiO3A compound having a perovskite structure; whereas many of the synthetic perovskite-type compounds in the field of materials science have widely variable electrical propertiesSuch as insulators, semiconductors, high temperature superconductors, or have good ferroelectricity and piezoelectricity. Based on this, the research of perovskite structure compounds has very important significance.
Barium titanate BaTiO3As another representative substance of perovskite compounds, there are such characteristics that: when it is stressed to change shape, it generates an electric current, which, upon energization, changes shape. When barium titanate is put in ultrasonic wave, it generates current under pressure, and the intensity of ultrasonic wave can be detected according to the magnitude of current generated by barium titanate. On the contrary, by passing a high frequency current through it, ultrasonic waves can be generated. Barium titanate is used in almost all ultrasonic instruments today. Meanwhile, barium titanate also has the characteristics of ferroelectric, piezoelectric, dielectric and the like, is an important electronic ceramic material, and is widely applied to the field of manufacturing various electronic components, such as high-capacity capacitors, monolithic capacitors, thermosensitive elements, pressure-sensitive elements, other sensitive elements and the like.
However, barium titanate is expensive and difficult to purify, and cannot meet the requirement of electronic ceramic materials on high-end substrates, and barium titanate is difficult to disperse and often has a caking phenomenon, which greatly affects the application of the materials.
Artificial fluorophlogopite (KMg)3(A1Si3O10)F2Also called synthetic mica) is a layered silicate compound which is prepared by high-temperature reaction, melting, cooling, crystallization and growth of chemical raw materials and high-quality mineral raw materials. The artificially synthesized fluorophlogopite sheet has the following characteristics: does not contain hydroxyl, so the temperature resistance is better; the insulating property is good; the compound is directly fired, so that the high-purity white pigment has high purity and whiteness.
Because the artificially synthesized fluorophlogopite powder is a flaky crystal and has high purity, the artificially synthesized fluorophlogopite powder can be used as a carrier of a barium titanate material, so that the use cost of the barium titanate material can be reduced, the use particle size of the barium titanate can be controlled, and the agglomeration phenomenon can be prevented. The synthetic mica powder is a pure chemical substance, has no heavy metal and impurity, can not affect the performance of barium titanate except the action of a carrier, can also enhance the spreading effect of the material, and is beneficial to the application of the barium titanate material in the fields of electronic ceramic materials and the like.
Disclosure of Invention
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a barium titanate-artificially synthesized fluorophlogopite composite material specifically comprises the following steps:
s1, adding 1250-mesh 80g of synthetic mica powder into 500ml of distilled water or deionized water, stirring for 0.5h (the rotating speed of a stirrer is 300-;
s2, preparing 2mol/LTiCl in advance4Solution, 2mol/LBaCl2Taking 100ml of solution, and dripping BaCl in advance2After 1-5ml of solution, the remaining BaCl was added2Solution, TiCl4Simultaneously dripping the solution and 10% NaOH solution into the reaction kettle of the step S1;
TiCl4dropping rate of solution and BaCl2The solution was the same and was about the NaOH solution addition rate 1/2. TiCl (titanium dioxide)4Solution, BaCl2The solution is dripped at constant speed by a metering pump, the NaOH solution is automatically dripped at constant speed by the metering pump, and the dripping amount of the NaOH solution is controlled by a pH controller (controlling the pH value to be about 1.8-2.0) to assist TiCl4Solution, BaCl2Reacting the solution in the synthetic mica powder solution;
s3, observing the change of the surface appearance of the synthetic mica powder (from silk white to milky white) until TiCl4Solution and BaCl2After the solution is added dropwise, stopping adding the NaOH solution, stirring at constant temperature and constant pH value for half an hour, adding distilled water or deionized water for suction filtration, and drying for 24 hours; finally obtaining BaTiO3/SynMica/BaTiO3And (3) composite powder.
The TiCl4The preparation method comprises the following steps:
adding a certain amount of water or ice (0-4 ℃) into a 500ml beaker in a ventilated place, and stirring by an electric stirrer; pipette a defined amount of 200ml TiC14Slowly adding dropwise into the fireA cup; the dilution concentration is about 2 mol/L; controlling the system temperature and acidity in the dilution process to TiC14After the solution was diluted uniformly, a clear solution was obtained which was slightly yellow and poured into a glass bottle for further use.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the barium titanate material with the perovskite structure is deposited and generated on the surface of the synthetic mica powder for the first time, so that the barium titanate is endowed with higher purity and controllable particle size, and the application field and material using effect of the barium titanate material are increased. Due to the carrier effect of the synthetic mica powder, the use cost of the barium titanate material is reduced, so that the novel composite material has very good market potential.
Drawings
FIG. 1 is a schematic flow chart 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 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 uses TiCl through liquid phase deposition method4、BaCl2Adding NaOH into a reaction kettle filled with synthetic mica powder in a certain dripping mode, and reacting to form nano-scale BaTiO under the conditions of controlling temperature and PH value3Depositing on the surface of the synthetic mica powder, dehydrating and washing to finally obtain the barium titanate-artificially synthesized fluorophlogopite composite material. The reaction equation is as follows:
TiCl4+ H2O = TiOCl2+ 2HCl
TiOCl2+ BaCl2+ 4NaOH = BaTiO3+ 4NaCl+ 2H2O
BaTiO3+ SynMica constant temperature, constant pH BaTiO3/SynMica/BaTiO3
Example one
A preparation method of a barium titanate-artificially synthesized fluorophlogopite composite material specifically comprises the following steps:
s1, adding 1250-mesh 80g of synthetic mica powder into 500ml of distilled water or deionized water, stirring for 0.5h (the rotating speed of a stirrer is 300-;
s2, preparing 2mol/LTiCl in advance4Solution, 2mol/LBaCl2Taking 100ml of solution, and dripping BaCl in advance2After 1-5ml of solution, the remaining BaCl was added2Solution, TiCl4The solution and 10% NaOH solution are added dropwise into the reaction kettle of step S1 at the same time.
TiCl4Dropping rate of solution and BaCl2The solution was the same and was about the NaOH solution addition rate 1/2. TiCl (titanium dioxide)4Solution, BaCl2The solution is dripped at constant speed by a metering pump, the NaOH solution is automatically dripped at constant speed by the metering pump, and the dripping amount of the NaOH solution is controlled by a pH controller (controlling the pH value to be about 1.8-2.0) to assist TiCl4Solution, BaCl2Reacting the solution in the synthetic mica powder solution;
s3, observing the change of the surface appearance of the synthetic mica powder (from silk white to milky white) until TiCl4Solution and BaCl2After the solution is added dropwise, stopping adding the NaOH solution, stirring at constant temperature and constant pH value for half an hour, adding distilled water or deionized water for suction filtration, and drying for 24 hours; finally obtaining BaTiO3/SynMica/BaTiO3And (3) composite powder.
TiCl in the above example4Preparing a solution:
adding a certain amount of water or ice (0-4 ℃) into a 500ml beaker in a ventilated place, and stirring by an electric stirrer; pipette a defined amount of 200ml TiC14Slowly dripping into a beaker; the dilution concentration is about 2 mol/L; controlling the system temperature and acidity in the dilution process to TiC14After the solution was diluted uniformly, a clear solution was obtained which was slightly yellow and poured into a glass bottle for further use.
In the condition of ice water bath and strong acid medium, TiCl4The hydrolysis of (a) may be carried out in three steps:
Figure 898719DEST_PATH_IMAGE001
the hydrolysis reaction (1) is a rapid reaction of TiCl4Dissolving in water at 0-4 deg.C to determine pH value satisfying the relation of formula (1). And ionization (2) and hydrolysis (3) are endothermic reactions, so that the temperature is reduced, the reactions (2) and (3) can be inhibited, and the generation of titanium dioxide as an impurity is avoided. According to the preparation conditions, an ice-water mixture is selected to be used as an ice-water bath. Control of TiCl4The hydrolysis temperature is 0-4 deg.C, and stirring with electric stirrer to make the temperature distribution of the system uniform.
In order to obtain pure titanium source and thus ensure high purity and good quality of the product, the TiCl is strictly controlled4Conditions of the solution formulation process. The invention aims to prepare high-quality nano barium titanate with high purity and uniform distribution, the molar ratio of Ba to Ti is close to 1, the nano barium titanate is deposited on the surface of the synthetic mica powder, and the control of the conditions is particularly important.
The invention is not limited to selecting the synthetic mica powder KMg3(A1Si3O10)F2The structure of the mica can also be selected from other platy mica substances, such as natural muscovite, phlogopite, lepidolite and the like.
The particle size of the synthetic mica powder is selected to be between 3000 meshes and 400 meshes, preferably 1250 meshes, and is determined according to the requirement of the barium titanate on the use particle size.
The NaOH solution is only used for adjusting the pH value of the reaction, and other alkaline solutions can be selected and used, and the NaOH solution is not limited to the NaOH solution.
Barium to titanium molar ratio (BaCl) during the reaction2：TiCl4) Is 1: 1.
The reaction process is carried out in ice water bath (0-4 deg.C) and pH value is 1.8-2.0, and the preferable conditions are as follows: t = 4 ℃, pH 1.8.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (8)

1. A preparation method of a barium titanate-artificially synthesized fluorophlogopite composite material is characterized by comprising the following steps:
s1, adding 1250-mesh 80g of synthetic mica powder into 500ml of distilled water or deionized water, stirring for 0.5h at the temperature of 0-4 ℃, wherein the rotating speed of a stirrer is 300-;
s2, preparing 2mol/LTiCl in advance4Solution, 2mol/LBaCl2Taking 100ml of solution, and dripping BaCl in advance2After 1-5ml of solution, the remaining BaCl was added2Solution, TiCl4Simultaneously dripping the solution and 10% NaOH solution into the reaction kettle of the step S1;
TiCl4dropping rate of solution and BaCl2The solutions were the same and were about the NaOH solution dropping rate 1/2; TiCl (titanium dioxide)4Solution, BaCl2The solution is dripped at constant speed through a metering pump, the NaOH solution is automatically dripped at constant speed through the metering pump, the pH value is controlled to be 1.8-2.0 through a pH controller, and the dripping amount of the NaOH solution is controlled to assist TiCl4Solution, BaCl2Reacting the solution in the synthetic mica powder solution;
s3, changing the surface appearance of the synthetic mica powder from silk white to milky white until TiCl4Solution and BaCl2After the solution is added dropwise, stopping adding the NaOH solution, stirring at constant temperature and constant pH value for half an hour, adding distilled water or deionized water for suction filtration, and drying for 24 hours; finally obtaining BaTiO3/SynMica/BaTiO3And (3) composite powder.
2. The method of claim 1, wherein TiCl is added to the barium titanate-synthetic fluorophlogopite composite material4The preparation method comprises the following steps:
adding a certain amount of water or ice into a 500ml beaker in a ventilated place, and stirring by using an electric stirrer; pipette a defined amount of 200ml TiC14Slowly dripping into a beaker; the dilution concentration is about 2 mol/L; controlling the system temperature and acidity in the dilution process to TiC14After the solution was diluted uniformly, a clear solution was obtained which was slightly yellow and poured into a glass bottle for further use.
3. The method of claim 2, wherein TiCl is added to the barium titanate-synthetic fluorophlogopite composite material4In the preparation method, the temperature of adding water or ice is 0-4 ℃.
4. The method for preparing barium titanate-artificially synthesized fluorophlogopite composite material according to claim 1, wherein the synthesized mica powder is KMg3(A1Si3O10)F2The synthetic mica powder with the structure.
5. The method for preparing a barium titanate-artificially synthesized fluorophlogopite composite material according to claim 1, wherein the particle size of the synthetic mica powder is between 3000 meshes and 400 meshes.
6. The method of claim 5, wherein the particle size of the synthetic mica powder is 1250 mesh.
7. The method for preparing a barium titanate-artificially synthesized fluorophlogopite composite material according to claim 1, wherein the molar ratio of barium to titanium in the reaction process is 1: 1.
8. The method for preparing a barium titanate-artificially synthesized fluorophlogopite composite material according to claim 1, wherein the reaction process is carried out at a temperature of T-4 ℃ and a pH of 1.8.
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