CN101333000B - Process for synthesizing high pure electronic grade barium titanate by liquid phase method - Google Patents
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- CN101333000B CN101333000B CN2007100525584A CN200710052558A CN101333000B CN 101333000 B CN101333000 B CN 101333000B CN 2007100525584 A CN2007100525584 A CN 2007100525584A CN 200710052558 A CN200710052558 A CN 200710052558A CN 101333000 B CN101333000 B CN 101333000B
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Abstract
The invention relates to a technique for synthesizing high-purity electronic grade barium titanate by a liquid phase method, which includes the following steps: oxalic acid is dissolved in deionized water, and barium chloride accounting for 2% of molar weight of oxalic acid is added in; the barium-titanium mixed solution is added into oxalic acid solution at the flow speed of 1.3-1.5m <3>/h for reaction; the obtained solid is put in a kiln for constant temperature calcination which lasts for 2-4 hours, then is taken out and processed by jet milling, placed in the kiln once more for secondary constant temperature calcination which lasts for 1-3 hours, and taken out for secondary jet milling and barium titanate powder is obtained finally. The barium titanate prepared by the invention has high purity, good dispersibility, uniform powder particle appearance and reasonable particle size. Therefore, the technique of the invention can solve the problem that the barium titanate powder prepared by the traditional method; more particularly, the existing coprecipitation method has sulphate impurities, severe glomeration, and the like, and can completely meet the requirements of the production of high-performance electronic components like base metal porcelain capacitors, etc.
Description
Technical field
The present invention relates to a kind of preparation technology of barium titanate, especially relate to a kind of technology of synthesizing high pure electronic grade barium titanate by liquid phase method.
Background technology
Barium carbonate powder be used for producing electronic components such as chip MLCC electric capacity, PTC element, probe, dielectric amplifier dielectric substance, be one of most important material in the electronic industry.The domestic production barium carbonate powder mainly contains methods such as solid phase method, liquid phase method at present.Wherein solid phase method is with BaCO
3And TiO
2Mix,, obtain barium carbonate powder after pulverizing then through high-temperature calcination more than 1200 ℃.Though solid phase method has advantages such as technology, equipment is simple, raw material is easy to get, its product impurity is many, and granularity is big, reactive behavior is low.
Liquid phase method comprises coprecipitation method and hydrothermal method, wherein coprecipitation method is present widely used a kind of method, this method is mixed solubility barium, titanium compound, add precipitation agent (oxalic acid, carbonate etc.) then, make barium, titanium compound produce co-precipitation, will obtain barium carbonate powder after throw out separation, drying, the calcining.Because in the coprecipitation method, they are many to be precipitation agent with oxalic acid, so this method oxalate precipitation method (abbreviation Oxalic Acid Method) that is otherwise known as.Though Oxalic Acid Method is eager to excel in whatever one does more a lot of than solid phase method synthetic barium titanate reactive behavior, its reunion is more serious, and is dispersed bad, particularly can not be used to make base metal (nickel electrode) ceramic condenser.When the barium titanate medium porcelain powder that adopts existing Oxalic Acid Method to produce was made the base metal cermet electrical condenser, the interior electrode of its electrical condenser will produce fusion (as shown in Figure 3) phenomenon, thereby caused condenser capacity to be disperseed, and insulation descends, so that can not use.
At present, the barium carbonate powder of tradition Oxalic Acid Method preparation generally can only be used for PTC element, noble metal electrode ceramic condenser (PME-MLCC) etc. raw materials quality is required not too high electronic ceramic fields, and can not be used to make the electrodes in base metal ceramic condenser (BME-MLCC) higher to the barium carbonate powder specification of quality.
Summary of the invention
Technical problems such as the present invention solves the prior art barium titanate to produce existing powder purity low, and the big and size-grade distribution of particle is inhomogeneous.
The present invention has also solved existing coprecipitation method simultaneously, especially the barium carbonate powder produced of the Oxalic Acid Method technical problem that can not be used to make electrodes in base metal ceramic condenser (BME-MLCC).To provide a kind of is the technology of the synthesizing high pure electronic grade barium titanate by liquid phase method of precipitation agent with oxalic acid.
The present invention is mainly solved the problems of the technologies described above by following technical proposals: it may further comprise the steps:
A. bariumchloride is dissolved in the deionized water, is mixed with the barium chloride solution of 1.0-1.3mol/L; The titanium tetrachloride dissolution in low temperature in deionized water, is mixed with titanium tetrachloride (the dichloro oxygen titanium) aqua liquid of 1.5-2.5mol/L; Measure according to the mol ratio of Ba/Ti 1.05 the ratio of being not less than then, solution after the above-mentioned metering is mixed in the same container, after stirring, add proper amount of deionized water, the mixing solutions that is mixed with concentration and is 0.5mol/L is standby;
B. oxalic acid is dissolved in the deionized water, and adds the bariumchloride of oxalic acid molar weight 2%, filtering throw out then is mixed with the oxalic acid solution of 1.1-1.2mol/L; Then the oxalic acid solution temperature is heated to 50-70 ℃, under intense stirring condition, adds the polyoxyethylene glycol of oxalic acid solution gross weight 2-3 ‰, simultaneously with barium titanium mixing solutions with 1.3-1.5m
3The flow velocity of/h is added in the oxalic acid solution and reacts, and during reaction, its temperature of reaction continues to be controlled at 50-70 ℃, add material after 30 minutes, to obtain titanium oxyoxalate precipitated barium slurry and put into whizzer, and add water and wash, when detecting the washing electrical conductivity of water less than 20 μ s/cm
2The time, just obtain highly purified barium titanium oxalate solid after the drying;
C. the solid that step b is obtained is put into kiln and is calcined, and calcining temperature is controlled at 800-1000 ℃, and calcining at constant temperature was taken out and carried out comminution by gas stream after 2-4 hours; Then put into kiln again and carry out the calcining second time, calcining temperature is controlled at 1060-1150 ℃, calcining at constant temperature was taken out and is carried out the comminution by gas stream second time after 1-3 hours, obtained barium carbonate powder at last.
The contriver finds by a large amount of experiments: in traditional co-precipitation method-Oxalic Acid Method technology, owing to contain a spot of sulfate ion in its precipitation agent oxalic acid solution, therefore can produce vitriol when the preparation barium titanate and mix in wherein.Because the base metal cermet electrical condenser is that sintering forms in reducing atmosphere with electrode size (nickel slurry) by medium porcelain powder (main raw material is a barium titanate), like this when sintered nickel electrode porcelain powder, miscellaneous vitriol decomposes in its reducing atmosphere in the barium titanate, nickel powder generation chemical reaction during the product of its decomposition (sulphur compound) is starched with nickel easily, the electrode fusing point descends and melts in causing, thereby influences the quality of nickel electrode electrical condenser.Technology of the present invention is before coprecipitation reaction, being about to a spot of bariumchloride earlier is added in the oxalic acid solution, with the formation barium sulfate precipitate, thereby the sulfate ion in the oxalic acid solution is thoroughly removed, in the technology of follow-up preparation barium titanate, just can not produced sulfate impurities like this.
Therefore, when adopting the barium titanate of this law preparation to starch sintering with nickel, chemical reaction can not take place, finally allow the interior electrode in the medium porcelain powder be able to complete formation, thereby guaranteed the quality of production of electrical condenser.
Polyoxyethylene glycol of the present invention is a kind of nonionogenic tenside, and behind a spot of polyoxyethylene glycol of adding, the barium titanium oxalate deposit seeds good dispersity that can allow the reaction of barium titanium mixing solutions and oxalate co-precipitation be produced is not reunited in the oxalic acid solution.
The present invention adopts secondary clacining and disintegrating process when calcining, the barium carbonate powder purity height that makes preparation, and good dispersity, and the powder granule pattern is single, reasonable particle size.Thereby overcome traditional method, the barium carbonate powder of particularly existing Oxalic Acid Method preparation has sulfate impurities, the problem such as serious of reuniting, and therefore can satisfy the needs of producing the contour performance electronic component of base metal cermet electrical condenser fully.
Description of drawings
Fig. 1 is the electron micrograph of barium titanate of the present invention (0.2-0.3 ц m);
Fig. 2 is the electron micrograph of barium titanate of the present invention (0.4-0.5 ц m).
Fig. 3 is the cross sectional photograph that the barium carbonate powder of traditional Oxalic Acid Method preparation is made the nickel electrode ceramic condenser.
Fig. 4 is the cross sectional photograph that the barium carbonate powder for preparing of the present invention is made the nickel electrode ceramic condenser.
Embodiment
Below by embodiment, and in conjunction with the accompanying drawings, technical scheme of the present invention is described in further detail.
Embodiment 1: bariumchloride is dissolved in the deionized water, is mixed with the barium chloride solution of 1.0mol/L; Titanium tetrachloride in 35 ℃ of dissolving deionized waters, is mixed with the titanium tetrachloride aqua liquid of 2.0mol/L; Measure 0.5 liter of 1.05 liters of above-mentioned barium chloride solutions and titanium tetrachloride aqua liquid respectively with graduated cylinder then, place same container, and adding 0.45 liter of deionized water and stirring, to make barium titanium mixing solutions after mix standby; 2.2mol oxalic acid is dissolved in the 2L deionized water, the bariumchloride that adds oxalic acid molar weight 2% stirs, filtering throw out then, be mixed with the oxalic acid solution of 1.1mol/L, then the oxalic acid solution temperature is heated to 60 ℃, under intense stirring condition, add the polyoxyethylene glycol of oxalic acid solution gross weight 2 ‰, simultaneously with barium titanium mixing solutions with 0.4m
3The flow velocity of/h is added in the oxalic acid solution and reacts; During reaction, its temperature of reaction continues to be controlled at 60 ℃, adds material after 30 minutes, will obtain titanium oxyoxalate precipitated barium slurry and put into whizzer, adds water and washs, and is lower than 20 μ s/cm when detecting the washing electrical conductivity of water
2The time, dry; The solid that obtains is put into kiln to be calcined, calcining temperature is controlled at 800 ℃, after the calcining at constant temperature 4 hours, comminution by gas stream is carried out in taking-up, then put into kiln again and carry out the calcining second time, calcining temperature is controlled at 1060 ℃, calcining at constant temperature is after 1 hour, the comminution by gas stream second time is carried out in taking-up, obtains purity height, monodispersed barium carbonate powder at last.Stereoscan photograph (8000 times) shows that this morphology microstructure is complete, and particle diameter is 0.2-0.3 ц m, and good dispersity, does not have agglomeration, as shown in Figure 1.
Embodiment 2: bariumchloride is dissolved in the deionized water, is mixed with the barium chloride solution of 1.2mol/L; Titanium tetrachloride in 35 ℃ of dissolving deionized waters, is mixed with the titanium tetrachloride aqua liquid of 1.5mol/L; Measure 0.583 liter of 0.875 liter of above-mentioned barium chloride solution and titanium tetrachloride aqua liquid respectively with graduated cylinder then, place same container, and adding 0.542 liter of deionized water and stirring, to make barium titanium mixing solutions after mix standby; 2.2mol oxalic acid is dissolved in the 2L deionized water, and the bariumchloride that adds oxalic acid molar weight 2% stirs, and filtering throw out then is mixed with the oxalic acid solution of 1.1mol/L; Then the oxalic acid solution temperature is heated to 50 ℃, under intense stirring condition, adds the polyoxyethylene glycol of oxalic acid solution gross weight 3 ‰, simultaneously with barium titanium mixing solutions with 0.5m
3The flow velocity of/h is added in the oxalic acid solution and reacts; During reaction, its temperature of reaction continues to be controlled at 50 ℃, after 30 minutes, will obtain titanium oxyoxalate precipitated barium slurry and put into whizzer, adds water and washs, and is lower than 20 μ s/cm when detecting the washing electrical conductivity of water
2The time, dry; The solid that obtains is put into kiln calcine, calcining temperature is controlled at 1000 ℃, calcining at constant temperature was taken out and is carried out comminution by gas stream after 3 hours; Then put into kiln again and carry out the calcining second time, calcining temperature is controlled at 1150 ℃, calcining at constant temperature was taken out and is carried out the comminution by gas stream second time after 2 hours, obtained purity height, monodispersed barium carbonate powder at last.Stereoscan photograph (8000 times) shows that this morphology microstructure is complete, and particle diameter is 0.4-0.5 ц m, and good dispersity, does not have agglomeration, as shown in Figure 2.
Embodiment 3: bariumchloride is dissolved in the deionized water, is mixed with the barium chloride solution of 1.3mol/L; Titanium tetrachloride in 35 ℃ of dissolving deionized waters, is mixed with the titanium tetrachloride aqua liquid of 2.5mol/L; Measure 0.83 liter of 0.77 liter of above-mentioned barium chloride solution and titanium tetrachloride aqua liquid respectively with graduated cylinder then, it is standby to make barium titanium mixing solutions after the mixing; 2.2mol oxalic acid is dissolved in the 1.83L deionized water, and the bariumchloride that adds oxalic acid molar weight 2% stirs, and filtering throw out then is mixed with the oxalic acid solution of 1.2mol/L; Then the oxalic acid solution temperature is heated to 70 ℃, under intense stirring condition, adds the polyoxyethylene glycol of oxalic acid solution gross weight 2 ‰, simultaneously with barium titanium mixing solutions with 0.3m
3The flow velocity of/h is added in the oxalic acid solution and reacts, and during reaction, its temperature of reaction continues to be controlled at 70 ℃, add material after 30 minutes, to obtain titanium oxyoxalate precipitated barium slurry and put into whizzer, and add water and wash, be lower than 20 μ s/cm when detecting the washing electrical conductivity of water
2The time, dry; The solid that obtains is put into kiln to be calcined, calcining temperature is controlled at 900 ℃, after the calcining at constant temperature 2 hours, comminution by gas stream is carried out in taking-up, then put into kiln again and carry out the calcining second time, calcining temperature is controlled at 1100 ℃, calcining at constant temperature is after 3 hours, the comminution by gas stream second time is carried out in taking-up, obtains purity height, monodispersed barium carbonate powder at last.Stereoscan photograph (8000 times) shows that this morphology microstructure is complete, and particle diameter is 0.3-0.4 ц m, and good dispersity, does not have agglomeration.
Fig. 3 is the cross sectional photograph of making the nickel electrode ceramic condenser with the barium carbonate powder of traditional Oxalic Acid Method preparation.As can be seen from the figure, its nickel electrode fusion is serious, and each electrode interface is fuzzy, has occurred hole.
Fig. 4 is the cross sectional photograph that adopts the barium carbonate powder making nickel electrode ceramic condenser of the present invention's preparation.As can be seen from the figure, its nickel electrode is complete, and each electrode interface is clear, does not have melting phenomenon.
Claims (1)
1. the technology of a synthesizing high pure electronic grade barium titanate by liquid phase method is characterized in that may further comprise the steps in described technology:
A. bariumchloride is dissolved in the deionized water, is mixed with the barium chloride solution of 1.0-1.3mol/L; With titanium tetrachloride in 35 ℃ of dissolution in low temperature in deionized water, be mixed with the titanium tetrachloride aqua liquid of 1.5-2.5mol/L; Be that 1.05 ratio is measured according to the mol ratio of Ba/Ti then, solution after the above-mentioned metering is mixed in the same container, after stirring, add proper amount of deionized water, the mixing solutions that is mixed with concentration and is 0.5mol/L is standby;
B. oxalic acid is dissolved in the deionized water, and adds the bariumchloride of oxalic acid molar weight 2%, filtering throw out then is mixed with the oxalic acid solution of 1.1-1.2mol/L; Then the oxalic acid solution temperature is heated to 50-70 ℃, under intense stirring condition, the polyoxyethylene glycol that adds oxalic acid solution gross weight 2-3 ‰, simultaneously barium titanium mixing solutions is added in the oxalic acid solution with the flow velocity of 1.3-1.5m3/h and reacts, during reaction, its temperature of reaction continues to be controlled at 50-70 ℃, add material after 30 minutes, to obtain titanium oxyoxalate precipitated barium slurry and put into whizzer, and add water and wash, when detecting the washing electrical conductivity of water less than 20 μ s/cm
2The time, just obtain the barium titanium oxalate solid after the drying;
C. the solid that step b is obtained is put into kiln and is calcined, and calcining temperature is controlled at 800-1000 ℃, after calcining at constant temperature 2-4 hour, takes out and carries out comminution by gas stream; Then put into kiln again and carry out the calcining second time, calcining temperature is controlled at 1060-1150 ℃, after calcining at constant temperature 1-3 hour, take out and carry out the comminution by gas stream second time, obtain barium carbonate powder at last.
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| US20140221685A1 (en) * | 2011-04-01 | 2014-08-07 | M. Technique Co., Ltd. | Method for producing barium titanyl salt and barium titanate |
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| KR101104627B1 (en) * | 2009-06-11 | 2012-01-12 | 씨큐브 주식회사 | Barium titanate nano powder and method for fabricating the same |
| KR20120025431A (en) * | 2010-09-07 | 2012-03-15 | 니폰 가가쿠 고교 가부시키가이샤 | Barium titanyl oxalate particle, method for preparing the same and method for preparing barium titanate |
| CN101985395A (en) * | 2010-11-26 | 2011-03-16 | 天津师范大学 | Method for preparing high dielectric constant barium titanate ceramic |
| CN102093047B (en) * | 2011-01-04 | 2013-01-23 | 天津师范大学 | Sintering method for increasing dielectric constant of barium titanate |
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| CN114988868B (en) * | 2022-05-25 | 2023-07-21 | 大连大学 | Preparation method of strontium titanate ceramic with giant dielectric constant and low dielectric loss |
| CN116253564A (en) * | 2023-03-03 | 2023-06-13 | 重庆新申世纪新材料科技有限公司 | Preparation process of nanoscale tetragonal phase barium titanate powder |
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