CN103626223B - A kind of Barium metatitanate. production technology - Google Patents
A kind of Barium metatitanate. production technology Download PDFInfo
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- CN103626223B CN103626223B CN201310527776.4A CN201310527776A CN103626223B CN 103626223 B CN103626223 B CN 103626223B CN 201310527776 A CN201310527776 A CN 201310527776A CN 103626223 B CN103626223 B CN 103626223B
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Abstract
A kind of Barium metatitanate. production technology, it prepares metatitanic acid respectively after titanium tetrachloride depth hydrolysis in deionized water, dispersion；Barium hydroxide is configured to barium hydroxide solution.Then, after both being stirred, send in ultrasonic sprayer, carry out ullrasonic spraying thermal decomposition, finally prepared powder is carried out high-temperature calcination and prepare tetragonal-phase barium titanate.The present invention uses titanium tetrachloride and barium hydroxide to do raw material, by reasonably selecting process route, including realizing, prepared by precursor liquid, mixed aerosol, local behavior, powder are collected, washing is dried and the operation such as high-temperature calcination, achieve the batch production of Barium metatitanate., obtained Barium metatitanate. complete appearance, of fine qualities, meet the requirement that electronic device produces.Present invention improves the most methodical deficiency, there is good market prospect and economic benefit.
Description
Technical field
The present invention relates to a kind of electron ceramic material, especially relate to a kind of Barium metatitanate. production technology.
Background technology
Barium metatitanate. (BaTiO3), there are high-k and low dielectric loss, excellent pressure and insulating properties, be widely used in multi-layer ceramic capacitance MLCC, critesistor PTCR, electro-optical device and DRMA device etc., be described as the pillar of electronic ceramics industry.Can have five kinds of crystal structures during Barium metatitanate. solid-state, temperature is followed successively by from high to low: six sides, isometry, four directions, oblique side and trigonal system.In addition to isometry, remaining structure all presents ferroelectricity.In various types of Barium metatitanate .s, especially tetragonal-phase barium titanate is one of effective measures improving Barium metatitanate. electronic component performance.
Prepare Barium metatitanate. and mainly have a following methods: 1, solid phase method: it is by BaCO3And TiO2For raw material, mixed grinding, extruded after, high-temperature calcination obtains BaTiO3Powder body, but its mixing is uneven, and degree of grinding is big on reaction impact, causes that product granularity is uneven, purity is the highest；2, coprecipitation: it is in the metal salt solution of mixing, adds precipitant and obtains the mixed uniformly precipitation of Multiple components, then thermally decompose, and product purity is high, be evenly distributed, but technological process length, there is side reaction, easily induces one impurity；3, vapor phase method: this method uses metal chloride or metal alkoxide to be raw material, entered the modes such as electric arc, burning, induced with laser heat make material gasification or formed plasma, react through gas phase and be quenched in media as well and obtain Barium metatitanate., its product purity is high, be evenly distributed, but equipment is complicated, cost height.
Nebulization is the synthetic route that development in recent years is got up, and it belongs to vapor phase method category, is to do presoma with liquid solution, and raw material mixes under solution state, makes vaporific, then adds and is thermally generated fine powder, and its process is rapid, and component is uniform.But the preparation of precursor solution and process route select particular importance, otherwise make its granule of Barium metatitanate. be easily generated fragment, broken shell, and Porous hollow granule, these bad shape characteristics all can affect the performance of electronic device.
Summary of the invention
It is an object of the invention to provide a kind of Barium metatitanate. production technology, more complicated to improve the preparation of existing Barium metatitanate. precursor solution and technique, cause the phenomenons such as barium titanate particles fragment, broken shell, Porous hollow, the problems such as product quality is impacted.
The present invention mainly solves above-mentioned technical problem by following technical proposals: a kind of Barium metatitanate. production technology, comprises the following steps:
A. by titanium tetrachloride and deionized water in the ratio feeding of 1:0.67-1.5, titanium tetrachloride is slowly added in deionized water, make it dissolve, obtain the dichloro oxygen titanium solution of 0.25-0.4mol/L, it is warming up to 90-100 DEG C, add the dispersant of total solution weight 3-5% under stirring and hydrolyze 2-4 hour, obtaining metatitanic acid gel suspension, be subsequently adding the water diluted for use of metatitanic acid gel suspension equivalent weight；Described dispersant is that hydrolysis poly-maleic anhydride acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, maleic acid-acrylic acid copolymer are by the mixture of 3:1:1；
B. barium hydroxide is dissolved in plasma water, is configured to the barium hydroxide solution of 1.0-1.3 mol/L；
C. in the ratio metering that Ti:Ba mol ratio is 1:1-1.1, barium hydroxide solution is added in metatitanic acid suspension, quickly stirring, then mixing liquid is sent in ultrasonic nebulizer in 180-220 DEG C, and be passed through nitrogen that volume ratio is 2:1.5 and carry out ullrasonic spraying thermal decomposition with oxygen mixed gas, obtain pulverulent solids；
D. the powder of collection is washed with deionized 3 times, is dried 30 minutes in 280-320 DEG C in sending into vacuum drying oven, then powder is calcined 1-2 hour in 1000-1200 DEG C, obtain tetragonal-phase barium titanate.
As preferably, it is provided with blanking device bottom described ultrasonic nebulizer, ultrasonic nebulizer outer wall is provided with electric heater, ultrasonic nebulizer top is provided with aerochamber, is provided with ultrasonic atomization sheet bottom described aerochamber, and atomizing piece is connected with atomization control circuit, aerochamber top is provided with nozzle, this nozzle is connected with ultrasonic nebulizer top by pipeline, and the left side of aerochamber is provided with air inlet, and air inlet is connected with gas reservoir；The top of aerochamber is provided with inlet, and inlet is connected with solution reservoir by pipeline.
The present invention uses titanium tetrachloride and barium hydroxide to do raw material, by reasonably selecting process route, including realizing, prepared by precursor liquid, mixed aerosol, local behavior, powder are collected, washing is dried and the operation such as high-temperature calcination, achieve the batch production of Barium metatitanate., obtained Barium metatitanate. complete appearance, of fine qualities, meet the requirement that electronic device produces.Present invention improves the most methodical deficiency, there is good market prospect and economic benefit.
Accompanying drawing explanation
Fig. 1 is the structural representation of ultrasonic nebulizer；
Fig. 2 is the structural representation of aerochamber in Fig. 1；
Fig. 3 is the process chart of the present invention；
Fig. 4 is the electromicroscopic photograph that Barium metatitanate. prepared by the present invention amplifies 10,000 times；
Fig. 5 is the electromicroscopic photograph that Barium metatitanate. prepared by the present invention amplifies 20,000 times；
Fig. 6 is the electromicroscopic photograph that Barium metatitanate. prepared by the present invention amplifies 30,000 times；
Fig. 7 is the electromicroscopic photograph that Barium metatitanate. prepared by the present invention amplifies 40,000 times.
Detailed description of the invention
Below in conjunction with the accompanying drawings and detailed description of the invention, technical scheme is described further.
Fig. 1 is the structural representation of ultrasonic nebulizer, and Fig. 2 is the structural representation of aerochamber in Fig. 1, and Fig. 3 is the process chart of the present invention.As shown in the figure, it is provided with blanking device 1 bottom this ultrasonic nebulizer 20, ultrasonic nebulizer outer wall is provided with electric heater 2, ultrasonic nebulizer top is provided with the aerochamber 3 that can carry out ultrasonic atomization, is provided with ultrasonic atomization sheet 4 bottom aerochamber 3, and atomizing piece 4 is connected with atomization control circuit 5, aerochamber 3 top is provided with nozzle 6, this nozzle 6 is connected with ultrasonic nebulizer top by pipeline 7, and the left side of aerochamber 3 is provided with air inlet 8, and air inlet 8 is connected with gas reservoir 9；The top of aerochamber 3 is provided with inlet 10, and inlet 10 is connected with solution reservoir 11 by pipeline.
Prepare Barium metatitanate. can adopt with the following method:
Embodiment 1: a kind of Barium metatitanate. production technology, comprises the following steps:
A. by titanium tetrachloride and deionized water in the ratio feeding of 1:0.67, titanium tetrachloride is slowly added in deionized water, make it dissolve, obtain the dichloro oxygen titanium solution of 0.25mol/L, it is warming up to 90 DEG C, add the dispersant of total solution weight 3% under stirring and hydrolyze 2 hours, obtaining metatitanic acid gel suspension, be subsequently adding the water diluted for use of metatitanic acid gel suspension equivalent weight；Described dispersant is that hydrolysis poly-maleic anhydride acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, maleic acid-acrylic acid copolymer are by the mixture of 3:1:1；
B. barium hydroxide is dissolved in plasma water, is configured to the barium hydroxide solution of 1.0mol/L；
C. in the ratio metering that Ti:Ba mol ratio is 1:1, barium hydroxide solution is added in metatitanic acid suspension, quickly stirring, then mixing liquid is sent in ultrasonic nebulizer in 180 DEG C, and be passed through nitrogen that volume ratio is 2:1.5 and carry out ullrasonic spraying thermal decomposition with oxygen mixed gas, obtain pulverulent solids；
D. the powder of collection is washed with deionized 3 times, is dried 30 minutes in 280 DEG C in sending into vacuum drying oven, then powder is calcined 2 hours in 1000 DEG C, obtain tetragonal-phase barium titanate.
Embodiment 2: a kind of Barium metatitanate. production technology, comprises the following steps:
A. by titanium tetrachloride and deionized water in the ratio feeding of 1:1.08, titanium tetrachloride is slowly added in deionized water, make it dissolve, obtain the dichloro oxygen titanium solution of 0.32mol/L, it is warming up to 95 DEG C, add the dispersant of total solution weight 4% under stirring and hydrolyze 3 hours, obtaining metatitanic acid gel suspension, be subsequently adding the water diluted for use of metatitanic acid gel suspension equivalent weight；Described dispersant is that hydrolysis poly-maleic anhydride acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, maleic acid-acrylic acid copolymer are by the mixture of 3:1:1；
B. barium hydroxide is dissolved in plasma water, is configured to the barium hydroxide solution of 1.15 mol/L；
C. in the ratio metering that Ti:Ba mol ratio is 1:1.05, barium hydroxide solution is added in metatitanic acid suspension, quickly stirring, then mixing liquid is sent in ultrasonic nebulizer in 200 DEG C, and be passed through nitrogen that volume ratio is 2:1.5 and carry out ullrasonic spraying thermal decomposition with oxygen mixed gas, obtain pulverulent solids；
D. the powder of collection is washed with deionized 3 times, is dried 30 minutes in 300 DEG C in sending into vacuum drying oven, then powder is calcined 1.5 hours in 1100 DEG C, obtain tetragonal-phase barium titanate.
Embodiment 3: a kind of Barium metatitanate. production technology, comprises the following steps:
A. by titanium tetrachloride and deionized water in the ratio feeding of 1:1.5, titanium tetrachloride is slowly added in deionized water, make it dissolve, obtain the dichloro oxygen titanium solution of 0.4mol/L, it is warming up to 100 DEG C, add the dispersant of total solution weight 5% under stirring and hydrolyze 4 hours, obtaining metatitanic acid gel suspension, be subsequently adding the water diluted for use of metatitanic acid gel suspension equivalent weight；Described dispersant is that hydrolysis poly-maleic anhydride acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, maleic acid-acrylic acid copolymer are by the mixture of 3:1:1；
B. barium hydroxide is dissolved in plasma water, is configured to the barium hydroxide solution of 1.3 mol/L；
C. in the ratio metering that Ti:Ba mol ratio is 1:1.1, barium hydroxide solution is added in metatitanic acid suspension, quickly stirring, then mixing liquid is sent in ultrasonic nebulizer in 220 DEG C, and be passed through nitrogen that volume ratio is 2:1.5 and carry out ullrasonic spraying thermal decomposition with oxygen mixed gas, obtain pulverulent solids；
D. the powder of collection is washed with deionized 3 times, is dried 30 minutes in 320 DEG C in sending into vacuum drying oven, then powder is calcined 1 hour in 1200 DEG C, obtain tetragonal-phase barium titanate.
Fig. 4, Fig. 5, Fig. 6, Fig. 7 part is not the Barium metatitanate. of embodiment 2 preparation, at accelerating potential 20KV, 10,000 times, 20,000 times, 30,000 times, the photo of 40,000 times is amplified respectively under the EVO Electronic Speculum of operating distance 6mm, that can clean from photo sees Barium metatitanate. structural integrity, does not has fragment, broken shell, hollow porous etc. bad.
The Barium metatitanate. product that embodiment 1-3 produces, by HG/T 3587-2009 " used in electronic industry high-purity Barium metatitanate. " analytical control, its assay is as follows:
As can be seen from the above data, the Barium metatitanate. indices using the present invention to prepare all has reached the requirement of used in electronic industry high-purity barium titanate HBT-05 grade, meets industrial needs.
Finally it is pointed out that above detailed description of the invention is only the more representational example of the present invention.It is clear that the invention is not restricted to above-mentioned detailed description of the invention, it is also possible to there are many deformation.Every any simple modification, equivalent variations and modification made above detailed description of the invention according to the technical spirit of the present invention, is all considered as belonging to protection scope of the present invention.
Claims (1)
1. a Barium metatitanate. production technology, is characterized in that this technique comprises the following steps:
A. by titanium tetrachloride and deionized water in the ratio feeding of 1:0.67-1.5, titanium tetrachloride is slowly added in deionized water, make it dissolve, obtain the dichloro oxygen titanium solution of 0.25-0.4mol/L, it is warming up to 90-100 DEG C, add the dispersant of total solution weight 3-5% under stirring and hydrolyze 2-4 hour, obtaining metatitanic acid gel suspension, be subsequently adding the water diluted for use of metatitanic acid gel suspension equivalent weight；Described dispersant is that hydrolysis poly-maleic anhydride acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, maleic acid-acrylic acid copolymer are by the mixture of 3:1:1；
B. barium hydroxide is dissolved in plasma water, is configured to the barium hydroxide solution of 1.0-1.3 mol/L；
C. in the ratio metering that Ti:Ba mol ratio is 1:1-1.1, barium hydroxide solution is added in metatitanic acid suspension, quickly stirring, then mixing liquid is sent in ultrasonic nebulizer in 180-220 DEG C, and be passed through nitrogen that volume ratio is 2:1.5 and carry out ullrasonic spraying thermal decomposition with oxygen mixed gas, obtain pulverulent solids；
D. the powder of collection is washed with deionized 3 times, is dried 30 minutes in 280-320 DEG C in sending into vacuum drying oven, then powder is calcined 1-2 hour in 1000-1200 DEG C, obtain tetragonal-phase barium titanate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105714234A (en) * | 2016-01-27 | 2016-06-29 | 苏州优优电容器制造有限公司 | Method for plasma spraying high-dielectric ceramics film on aluminum foil |
| CN106315667B (en) * | 2016-08-07 | 2018-08-14 | 淮安新能源材料技术研究院 | The method for preparing solid phase of porous barium titanate micro-nano particle ball |
| CN113912110A (en) * | 2021-10-27 | 2022-01-11 | 龙佰禄丰钛业有限公司 | Method for recovering titanium dioxide and hydrochloric acid from titanium tetrachloride tail gas absorption liquid |
| CN116271891B (en) * | 2023-05-24 | 2023-08-04 | 泸州聚购科技发展有限公司 | Atomizing device for barium titanate production |
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| CN101238069A (en) * | 2005-08-04 | 2008-08-06 | 韩华石油化学株式会社 | Process for preparing barium titanate |
| CN101177245A (en) * | 2007-11-21 | 2008-05-14 | 北京矿冶研究总院 | Preparation method of nanostructured oxide powder |
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