CN105329939A - Preparation method of size-controllable nanoscale cubic-phase super-fine barium titanate powder - Google Patents
Preparation method of size-controllable nanoscale cubic-phase super-fine barium titanate powder Download PDFInfo
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Abstract
The invention discloses a preparation method of size-controllable nanoscale cubic-phase super-fine barium titanate powder. Relatively cheap titanium tetrachloride is used for preparing a titanium precursor solution TiClO2 through hydrolysis, the precursor solution is dropwise added into a mineralizing agent and dispersant solution, and continuous stirring is performed to obtain a titanium precursor gel solution; then centrifugal gel washing is performed to remove chloride ions, the prepared H4TiO4 gel and barium hydroxide or barium nitrate are grinded and dispersed with water and a dispersant according to a certain proportion to prepare mixed dispersed slurry, the mixed dispersed slurry is put into a reaction kettle for hydrothermal reaction, and then washing and drying are performed to obtain the nanoscale cubic-phase super-fine barium titanate powder good in dispersion and centralized in particle size, the average particle size of the power is smaller than 100 nm, and the specific surface area is within the range of 12.5-15.0 m<2>/g.
Description
Technical field
The present invention relates to function ceramics starting material ultrafine powder and prepare technical field, particularly relate to a kind of nano level barium carbonate powder Nanoparticle technology of preparing.
Background technology
Barium carbonate powder material, is widely used in heat sensitive component, ferroelectric piezoelectric components and parts, laminated ceramic capacitor etc. and uses as dielectric materials.
Along with the high speed development of electronic information technology, the demand of the microminiaturization of various electronics accessory, lightweight, high performance and stabilization.Also supply falls short of demand thereupon to have the demand of the nano level barium titanate functional ceramic powder material of high-k, even being described as the pillar of electric function ceramic material, is also national strategy development and the Hot spots for development of nanotechnology and ultrafine powder technology and focus development direction in recent years.
Barium carbonate powder is different from the physical and chemical performance of other ceramic powder materials because having, and is prepared industry by electron trade and chemical raw material and nanosecond science and technology industry is paid close attention to.The features such as its salient features has high-k, low-dielectric loss, and electrical insulation capability is superior.And these physical and chemical performances are simultaneously also more and more harsher to the requirement of barium carbonate powder, especially to the crystalline structure of powder, size-grade distribution, granular size and purity have had more and more higher requirement, are also difficult point and the focus of the control of numerous R & D and manufacture.
In recent years along with deepening continuously of hydrothermal method is produced and industry, traditional oxalate precipitation method, solid sintering technology, sol-gel method all more and more can not meet electronics higher-end businesses product to the requirement of starting material powder.Increasing enterprise uses hydrothermal method to prepare favorable dispersity in R and D, and pattern is even, the nano level superfine barium carbonate powder that granularity is concentrated.Wherein in order to ensure barium titanate withstand voltage properties and the dielectric layer being prepared into even density, and guarantee the electric capacity content of electrical condenser, also just more and more harsher to the following requirement of barium carbonate powder.
(a) D50≤1um, and particle size distribution range is narrower, with D50≤0.01um for the best; Favorable dispersity in slurrying process, is easy to sinter molding;
B () grain crystalline is good, lattice defect is less, and pattern is spherical or is approximately spherical for good;
C () barium titanium is more best than scope between 0.997-1.001, be 1.000 for best with atomic molar ratio;
D () specific surface area is with>=12.5m
2/ g is good.
Therefore, if by traditional method, as although the oxalic acid precipitation method in patent CN1417162A can meet the wherein demand of conventional capacitive material and the requirement of purity, but its each purge process is consuming time, increase production cost, and because abrasive grains is very large, pattern is poor, size-grade distribution is not concentrated, and power consumption is large.And for example solve the tediously long problem of preparation process time with solid sintering technology in the mode of dinectly bruning in Japanese TDK house journal CN101428850A, but accomplish that above some and good condition control, still need the energy of at substantial.
Generally, oxalate coprecipitation method can obtain the Super-fine Barium Titanate of submicron order, and has company to adopt this method, but production process is more, and after the powder reuniting caused, particle is larger.The another kind of method solid sintering technology of powder serious agglomeration, is more difficult to obtain finely disseminated Super-fine Barium Titanate simultaneously.Sol-gel method to obtain the higher powder of nano level purity comparatively speaking, but because of its growth cycle long, cost is high and be difficult to widely popularize employing in scale processes.The present invention adopts to have begun one's study in recent years to prepare dispersed Super-fine Barium Titanate preferably with the hydrothermal method grown up, because of its control that hydrothermal reaction condition can obtain that crystal formation is complete, pattern is regular by one step, the high purity barium carbonate powder of size tunable and narrow distribution range, therefore be widely deployed and study, and scale is used for industry production
For obtaining a kind of even particle size, crystalline structure is stablized, and favorable dispersity, the barium carbonate powder particle that purity is high, present inventor has performed a large amount of experimental studies and exploration, and is successfully applied to the mass output of Industrial products.
Summary of the invention
The object of the present invention is to provide a kind of preparation method that can carry out particle size uniformity control and the good nano level superfine barium carbonate powder of crystal formation.
The technical scheme realizing the object of the invention is as follows, and a kind of preparation method of controllable nanon size level Emission in Cubic Super-fine Barium Titanate, comprises the following steps:
1) first by TiCl
4be hydrolyzed, prepare titanium precursor solution TiClO
2;
2) precursor solution is added dropwise in mineralizer solution, constantly stirs, obtain titanium precursors gelating soln;
3) titanium precursors gelating soln is carried out centrifuge washing, removing chlorion, obtained H
4tiO
4gel;
4) by obtained H
4tiO
4gel mixes with hydrated barta or nitrate of baryta, adds water and dispersion agent carries out grinding distribution, makes the dispersion slurries of mixing;
5) by the dispersion slurries of mixing, be placed in reactor, control its filling ratio, carry out hydro-thermal reaction 2-10h at 150-250 DEG C, obtained barium titanate slurry;
6) in barium titanate slurry, add water and dispersion agent, carry out washing with dry, obtain nano level Emission in Cubic Super-fine Barium Titanate.
Further, TiCl in described step 1)
4add water and dispersion agent is hydrolyzed, wherein said dispersion agent is ethanol, quadrol, triethylamine, ethylene glycol one or more, TiCl
4and dispersion agent mass ratio is (50-10): between 1.0.
Further, described mineralizer is ammoniacal liquor.
Further, described mineralizer and TiCl
4mass ratio is (1.0-4.0): 1.0.
Further, the mol ratio in barium source and titanium source is (2.05 ~ 1.1): (0.9 ~ 1.02).
Further, described reactor filling ratio is 60-85%.
Further, in step 4), in grinding dispersion agent, step 6), washing dispersion agent is the one in polyacrylamide, PAA, formic acid, acetic acid or ethanol.
The preparation method of a kind of controllable nanon size level Emission in Cubic Super-fine Barium Titanate of the present invention, have employed unique H
4tiO
4dispersion gel and barium source ground and mixed technique.To improve its reactive behavior and reaction rate, improve reaction production efficiency.Wherein main outstanding advantages is the following aspects: the first, by adopting comparatively cheap refining TiCl
4original solution is with dispersion agent and mineralizer for dispersion, and obtained gel primary particle particle diameter is nano level, has obvious cost advantage and reduces reaction activity advantage; Second, a large amount of excess of chloride ion can be removed in centrifuge washing mode to the gel of preparation, the powder reuniting caused with the salt bridge effect reduced in hydrothermal reaction process, simultaneously because add dispersion agent and mineralizer, its particle can be obtained in lower barium titanium is than proportioning raw materials and comparatively disperse less barium carbonate powder, increase substantially reaction efficiency and dispersion advantages; 3rd, the dispersion agent added and mineralizer, before reaction raw materials, effectively can suppress the particle aggregation in titanium source, can reduce the use consumption in barium source simultaneously, reduce production cost; 4th, alcohols dispersion agent is added in washing with drying process, Granular composite not only can be made more even, reduce and reunite, also provide good condition for the later stage prepares high-purity tetragonal-phase barium titanate superfine powder, also ensure that its excellent electric property for raw-material preparation process such as laminated body, capacitor and thin layer electric capacity.
Nano level barium carbonate powder prepared by the present invention, adopts the mode that hydrothermal method and the hot method of partial solvent combine, obtained barium carbonate powder, pure phase degree is high, good dispersity, narrow distribution range, crystallization degree is good, uniform particle sizes, also has superior ferroelectric, the performance such as dielectric, piezoelectricity simultaneously, can be widely used in function ceramics, electric transducer, non-linear varistor, ultracapacitor, the electronic element device materials such as thermistor.Secondly, nano level superfine cubic phase barium titanate powder of the present invention also has high sintering activity, can prepare crystal formation intact, uniform particles, the tetra phase barium titanate powder of good dispersity, has range of application widely and space in electrode component fields such as thin layer electric capacity base mateirals.The present invention has dropped on probation in enterprises, production cost is low, and production efficiency is high, has the very good market competitiveness and advantage.
Accompanying drawing explanation
Fig. 1 is the SEM figure of embodiment one product;
Fig. 2 is the SEM figure of embodiment two product;
Fig. 3 is the SEM figure of embodiment three products;
Fig. 4 is the SEM figure of embodiment four-product.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
Embodiment 1:
Take 2.0KgTiCl
4, in temperature of reaction lower than under 30 DEG C of conditions, slowly drop in the mixing solutions filling 4.0Kg deionized water and 40g dispersion agent ethanol under constantly stirring in a kettle., obtained faint yellow viscosity TiOCl
2the aqueous solution, the HCl gas that period produces carries out tail gas absorption by NaOH alkali lye, and the solution after tail gas absorption is carried out condensing crystal, obtained technical grade NaCl crystal.Then under temperature of reaction is less than 30 DEG C and agitation condition to TiOCl
2add mineralizer ammoniacal liquor 6.0Kg in the aqueous solution, make its NH
3h
2o:TiCl
4mass ratio is between 3.0:1.0, and reaction system final pH is between 8-12, and period forms white gum throw out.This throw out is carried out deionized water centrifuge washing and is less than 100ppm to chloride ion content.Subsequently by the white depositions after washing and Ba (OH)
28H
2o solid and water 15.0Kg, the mol ratio controlling barium source and titanium source, at 1.2:1.0, is placed in grinding machine for grinding 30min, after it fully mixes together, finally by above-mentioned pulp solution under lower than 30 DEG C of conditions with ammoniacal liquor and quadrol mixing and stirring, then mixed solution is loaded in reactor, 150 DEG C of reactions 10 hours, be cooled to room temperature, product is filtered, deionized water wash, 110 DEG C of dryings, obtains the BaTiO of 80-100nm
3powder, as shown in Figure 1, powder structure is Emission in Cubic, and granule-morphology is spherical, is uniformly dispersed, and distribution is concentrated, and specific surface area is greater than 12.5m
2/ g, barium titanium is than between 0.999-1.001.
Embodiment 2:
Take 2.0KgTiCl
4, in temperature of reaction lower than under 30 DEG C of conditions, slowly drop in the mixing solutions filling 4.0kg deionized water and ethanol 200g under constantly stirring in a kettle., obtained faint yellow viscosity TiOCl
2the aqueous solution, the HCl gas that period produces carries out tail gas absorption by NaOH alkali lye, and the solution after tail gas absorption is carried out condensing crystal, obtained technical grade NaCl crystal.Then under temperature of reaction is less than 30 DEG C and agitation condition to TiOCl
2add ammoniacal liquor 2.0Kg in the aqueous solution, make its NH
3h
2o:TiCl
4mass ratio at 1.0:1.0, reaction system final pH is between 8-12, and period forms white gum throw out.This throw out is carried out deionized water centrifuge washing and is less than 100ppm to chloride ion content.Subsequently by the white depositions after washing and Ba (OH)
28H
2o solid and water 15.0Kg, control the mol ratio in barium source and titanium source at 2.05:1.02, be placed in grinding machine for grinding 30min together, after it fully mixes, finally by above-mentioned pulp solution under lower than 30 DEG C of conditions with ammoniacal liquor and triethylamine mixing and stirring, ammoniacal liquor and grinding dispersion agent mass ratio control between 25:0.5, then mixed solution is loaded in reactor, 200 DEG C of reactions 6 hours, be cooled to room temperature, product is filtered, deionized water wash, 110 DEG C of dryings, obtain the BaTiO of 80-100nm
3powder, as shown in Figure 2, powder structure is Emission in Cubic, and granule-morphology is spherical, is uniformly dispersed, and distribution is concentrated, and specific surface area is greater than 12.7m
2/ g, barium titanium is than between 0.999-1.001.
Embodiment 3:
Take 2.0KgTiCl
4, in temperature of reaction lower than under 30 DEG C of conditions, slowly drop under constantly stirring in a kettle. and fill in the deionized water of 3.0Kg, obtained faint yellow viscosity TiOCl
2the aqueous solution, the HCl gas that period produces carries out tail gas absorption by NaOH alkali lye, and the solution after tail gas absorption is carried out condensing crystal, obtained technical grade NaCl crystal.Then under temperature of reaction is less than 30 DEG C and agitation condition to TiOCl
2add ammoniacal liquor 4.0Kg in the aqueous solution, make its NH
3h
2o:TiCl
4mass ratio is between 2.5:1.0, and its reaction system final pH is between 8-14, and period forms white gum throw out.This throw out is carried out deionized water centrifuge washing and is less than 50ppm to chloride ion content.Subsequently by the white depositions after washing and Ba (NO
3)
2solid and water 20.0Kg, control the mol ratio in barium source and titanium source at 1.1:0.9, be placed in grinding machine for grinding 60min together, after it fully mixes, finally above-mentioned pulp solution is mixed with ammoniacal liquor and quadrol under lower than 30 DEG C of conditions, ammoniacal liquor and grinding dispersion agent mass ratio control between 25:0.5, stir 1h, 100g hydrogen peroxide is slowly added again after stirring, then mixed solution is loaded in reactor, 250 DEG C of reactions 2 hours, be cooled to room temperature, product is filtered, with deionization and alcohol mixeding liquid washing, mixed solution mass ratio is 2:1, then 110 DEG C of dryings, obtain the BaTiO of 70-100nm
3powder, as shown in Figure 3, powder structure is Emission in Cubic, and particle is spherical, is uniformly dispersed, and distribution is concentrated, and specific surface area is greater than 13.2m
2/ g, barium titanium is than between 0.9985-1.002.
Embodiment 4:
Take 2.0KgTiCl
4, in temperature of reaction lower than under 30 DEG C of conditions, slowly drop under constantly stirring in a kettle. and fill in the deionized water of 3.5Kg, obtained faint yellow viscosity TiOCl
2the aqueous solution, the HCl gas that period produces carries out tail gas absorption by NaOH alkali lye, and the solution after tail gas absorption is carried out condensing crystal, obtained technical grade NaCl crystal.Then under temperature of reaction is less than 30 DEG C and agitation condition to TiOCl
2add ammoniacal liquor 8.0Kg in the aqueous solution, make its NH
3h
2o:TiCl
4mass ratio is between 4.0:1.0, and its reaction system final pH is between 8-14, and period forms white gum throw out.This throw out is carried out deionized water centrifuge washing and is less than 50ppm to chloride ion content.Subsequently by the white depositions after washing and Ba (NO
3)
2the lysate mixing of solid and water 20.0Kg, control the mol ratio of barium and titanium at 1.5:1.0, be placed in grinding machine for grinding 60min together, after it fully mixes, finally by above-mentioned pulp solution under lower than 30 DEG C of conditions with ammoniacal liquor and triethylamine mixing and stirring 1h, 120g hydrogen peroxide is slowly added again after stirring, then mixed solution is loaded in reactor, 250 DEG C of reactions 4 hours, be cooled to room temperature, product is filtered, with deionization and alcohol mixeding liquid washing, mixed solution mass ratio is 2.5:1, then 110 DEG C of dryings, obtain the BaTiO of 70-100nm
3powder, as shown in Figure 4, powder structure is Emission in Cubic, and particle is spherical, is uniformly dispersed, and distribution is concentrated, and specific surface area is greater than 13.2m
2/ g, barium titanium is than between 0.999-1.001.
The above is only preferred embodiment of the present invention, not does any pro forma restriction to the present invention; Any those of ordinary skill in the art, do not departing under technical solution of the present invention ambit, the Method and Technology content of above-mentioned announcement all can be utilized to make many possible variations and modification to technical solution of the present invention, or be revised as the Equivalent embodiments of equivalent variations.Therefore, every content not departing from technical solution of the present invention, according to technical spirit of the present invention to any simple modification made for any of the above embodiments, equivalent replacement, equivalence change and modification, all still belongs in the scope of technical solution of the present invention protection.
Claims (7)
1. a preparation method for controllable nanon size level Emission in Cubic Super-fine Barium Titanate, is characterized in that, comprise the following steps:
1) first by TiCl
4be hydrolyzed, prepare titanium precursor solution TiClO
2;
2) precursor solution is added dropwise in mineralizer solution, constantly stirs, obtain titanium precursors gelating soln;
3) titanium precursors gelating soln is carried out centrifuge washing, removing chlorion, obtained H
4tiO
4gel;
4) by obtained H
4tiO
4gel mixes with hydrated barta or nitrate of baryta, adds water and dispersion agent carries out grinding distribution, makes the dispersion slurries of mixing;
5) by the dispersion slurries of mixing, be placed in reactor, control its filling ratio, carry out hydro-thermal reaction 2-10h at 150-250 DEG C, obtained barium titanate slurry;
6) in barium titanate slurry, add water and dispersion agent, carry out washing with dry, obtain nano level Emission in Cubic Super-fine Barium Titanate.
2. the preparation method of a kind of controllable nanon size level Emission in Cubic Super-fine Barium Titanate according to claim 1, is characterized in that, TiCl in described step 1)
4add water and dispersion agent is hydrolyzed, wherein said dispersion agent is ethanol, quadrol, triethylamine, ethylene glycol one or more, TiCl
4and dispersion agent mass ratio is (50-10): between 1.0.
3. the preparation method of a kind of controllable nanon size level Emission in Cubic Super-fine Barium Titanate according to claim 1, is characterized in that: described mineralizer is ammoniacal liquor.
4. the preparation method of a kind of controllable nanon size level Emission in Cubic Super-fine Barium Titanate according to claim 1 or 3, is characterized in that: described mineralizer and TiCl
4mass ratio is (1.0-4.0): 1.0.
5. the preparation method of a kind of controllable nanon size level Emission in Cubic Super-fine Barium Titanate according to claim 1, is characterized in that: the mol ratio in barium source and titanium source is (2.05 ~ 1.1): (0.9 ~ 1.02).
6. the preparation method of a kind of controllable nanon size level Emission in Cubic Super-fine Barium Titanate according to claim 1, is characterized in that: described reactor filling ratio is 60-85%.
7. the preparation method of a kind of controllable nanon size level Emission in Cubic Super-fine Barium Titanate according to claim 1, is characterized in that: in step 4), in grinding dispersion agent, step 6), washing dispersion agent is the one in polyacrylamide, PAA, formic acid, acetic acid or ethanol.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106076239A (en) * | 2016-06-21 | 2016-11-09 | 南京宇热材料科技有限公司 | A kind of horizontal reacting device and production method |
| CN107555987A (en) * | 2017-09-07 | 2018-01-09 | 安徽中创电子信息材料有限公司 | A kind of submicron order barium carbonate powder Nanoparticle preparation method |
| CN109809468A (en) * | 2018-12-28 | 2019-05-28 | 南通奥新电子科技有限公司 | A kind of preparation method and applications of nano barium phthalate |
| WO2021047205A1 (en) * | 2019-09-12 | 2021-03-18 | 三达膜科技（厦门）有限公司 | Method for preparing ceramic nanofiltration membrane |
| CN114477273A (en) * | 2022-02-17 | 2022-05-13 | 重庆新申世纪新材料科技有限公司 | Hydrothermal preparation process of tetragonal phase nano barium titanate powder |
| CN114477275A (en) * | 2022-03-08 | 2022-05-13 | 天津泽希新材料有限公司 | Preparation method of novel spherical barium titanate |
| CN115259211A (en) * | 2022-07-18 | 2022-11-01 | 吉林大学 | Superfine BaTiO3Controllable preparation method of nano crystal |
| CN115924963A (en) * | 2022-12-14 | 2023-04-07 | 深圳先进电子材料国际创新研究院 | Preparation method for synthesizing tetragonal nano barium titanate by hydrothermal method, tetragonal nano barium titanate and application thereof |
| CN117509718A (en) * | 2023-12-13 | 2024-02-06 | 湖北展鹏电子材料有限公司 | Spherical-like nano barium titanate and preparation method thereof |
| CN118005072A (en) * | 2024-04-10 | 2024-05-10 | 杭州兴容科技有限公司 | Hydrothermal synthesis method of barium titanate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106076239A (en) * | 2016-06-21 | 2016-11-09 | 南京宇热材料科技有限公司 | A kind of horizontal reacting device and production method |
| CN107555987A (en) * | 2017-09-07 | 2018-01-09 | 安徽中创电子信息材料有限公司 | A kind of submicron order barium carbonate powder Nanoparticle preparation method |
| CN109809468A (en) * | 2018-12-28 | 2019-05-28 | 南通奥新电子科技有限公司 | A kind of preparation method and applications of nano barium phthalate |
| WO2021047205A1 (en) * | 2019-09-12 | 2021-03-18 | 三达膜科技（厦门）有限公司 | Method for preparing ceramic nanofiltration membrane |
| CN114477273A (en) * | 2022-02-17 | 2022-05-13 | 重庆新申世纪新材料科技有限公司 | Hydrothermal preparation process of tetragonal phase nano barium titanate powder |
| CN114477275B (en) * | 2022-03-08 | 2024-05-14 | 天津泽希新材料有限公司 | Preparation method of spherical barium titanate |
| CN114477275A (en) * | 2022-03-08 | 2022-05-13 | 天津泽希新材料有限公司 | Preparation method of novel spherical barium titanate |
| CN115259211A (en) * | 2022-07-18 | 2022-11-01 | 吉林大学 | Superfine BaTiO3Controllable preparation method of nano crystal |
| CN115259211B (en) * | 2022-07-18 | 2023-11-24 | 吉林大学 | Superfine BaTiO 3 Controllable preparation method of nanocrystals |
| CN115924963A (en) * | 2022-12-14 | 2023-04-07 | 深圳先进电子材料国际创新研究院 | Preparation method for synthesizing tetragonal nano barium titanate by hydrothermal method, tetragonal nano barium titanate and application thereof |
| CN117509718A (en) * | 2023-12-13 | 2024-02-06 | 湖北展鹏电子材料有限公司 | Spherical-like nano barium titanate and preparation method thereof |
| CN117509718B (en) * | 2023-12-13 | 2024-05-28 | 湖北展鹏电子材料有限公司 | Spherical-like nano barium titanate and preparation method thereof |
| CN118005072A (en) * | 2024-04-10 | 2024-05-10 | 杭州兴容科技有限公司 | Hydrothermal synthesis method of barium titanate |
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Application publication date: 20160217 |