CN108203298A - A kind of low temperature preparation method of electronic ceramics powder - Google Patents
A kind of low temperature preparation method of electronic ceramics powder Download PDFInfo
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- CN108203298A CN108203298A CN201611173805.1A CN201611173805A CN108203298A CN 108203298 A CN108203298 A CN 108203298A CN 201611173805 A CN201611173805 A CN 201611173805A CN 108203298 A CN108203298 A CN 108203298A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- 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
- C04B35/462—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 based on titanates
- C04B35/465—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 based on titanates based on alkaline earth metal titanates
- C04B35/468—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 based on titanates based on alkaline earth metal titanates based on barium titanates
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The present invention relates to a kind of preparation methods of the barium carbonate powder of high content of tetragonal phase.The present invention carries out the preparation of barium carbonate powder using hydrothermal synthesis method, after the completion of hydro-thermal reaction, is detached, washed, dried, and Barium Titanate nano-powder is made, then the powder of preparation is heat-treated, finally obtains the barium carbonate powder of high content of tetragonal phase.The technology is simple for process, easily manipulates, and powder high purity obtained, sintering activity is good, tetragonality is strong, is conducive to the preparation of high performance ceramic material.
Description
Technical field
The present invention relates to a kind of electronic ceramics raw powder's production technology, the barium titanate of more precisely high content of tetragonal phase
Raw powder's production technology.
Background technology
Barium titanate (BaTiO3, referred to as " BT ") and there is typical perovskite structure, there is high-k, low-dielectric loss
The features such as, there are excellent ferroelectricity, piezoelectricity, pressure resistance and insulation performance, be widely used in the making of Ceramic sensible devices, especially
Multilayer ceramic capacitor (MLCC).Micromation and high capacity are the main trends of following MLCC development, this is just needed in MLCC
On preparation process condition realize dielectric layer thin layer and lamination multiple stratification, and it is high-purity, grain size is small and uniform, tetragonal phase crystallize
It is the key technology for realizing above-mentioned target to spend high barium carbonate powder.
At present, the preparation method of industrialized barium carbonate powder has solid phase method, oxalate coprecipitation method and hydro-thermal method.Gu
Phase law technology is more ripe, raw material is cheap, yield is high, at low cost, but product purity is low, performance is unstable, surface-active is poor, group
Divide segregation, largely effect on the performance of electronic device；The reaction temperature of oxalate coprecipitation method is low, powder granule size is small, sintering
It is active high, but the foreign ions such as poor, bases precipitating reagent of consistency easily remain between product batches；Hydro-thermal method it is simple for process, anti-
Answer temperature low, the product chemical uniformity synthesized is good, grain development is complete, reunite less, granularity is controllable, but hydrothermal synthesis goes out
Barium titanate crystal grain in contain a large amount of proton defect so that cubic phase barium titanate is stabilized at room temperature, so can not
The preparation of barium titanate ceramics is directly used in, thus limits the industrialized production of hydrothermal synthesis barium carbonate powder.
Invention content
It is existing to overcome the object of the present invention is to provide a kind of barium carbonate powder of high content of tetragonal phase and preparation method thereof
Drawbacks described above existing for technology.The method of the present invention can prepare the rate of output and reach the metatitanic acid that 95%, tetragonality (c/a) reaches 1.009
Barium powder.So-called tetragonality refers to the content of tetragonal phase of barium titanate crystal, and generally with c/a, (c and a are in barium titanate lattice respectively
Crystallographic axis) value represent, by Rietveld refine method calculate, take (200) crystallographic plane diffraction peak, the bigger theorys of c/a under normal circumstances
Bright content of tetragonal phase is higher, and theoretically for c/a up to 1.01, the barium titanate tetragonality that general hydro-thermal method obtains is less than 1.008.
The preparation method of the barium carbonate powder of the present invention, using hydrothermal synthesis with being heat-treated the method being combined, tool
Body step is as follows：
1st, Ti (C are weighed respectively in the ratio that Ba/Ti molar ratios are 1.4~1.54H9O)4With Ba (OH)2·8H2O, by Ti
(C4H9O)4It is mixed with amount of the ethyl alcohol by volume for 1: 0.6~1.8, stirs evenly, obtain light yellow transparent liquid；
2nd, a certain amount of ammonium hydroxide and deionized water are taken, volume ratio 4: 5, after mixing, under agitation, slowly
It is added drop-wise to dropwise in above-mentioned transparency liquid, hydrolysis occurs, and leucosol is generated, after ammonium hydroxide dilution drips, in room
Continue to stir 15min under temperature,；
3rd, under 90 DEG C of water bath conditions, Ba (OH) is dissolved by heating2·8H2O, dissolved barium hydroxide solution and white is molten
Glue mixes, and is fitted into hydrothermal reaction kettle liner, and loading is 40%~70%, seals reaction kettle, is put into 100 DEG C~200 DEG C
It is reacted in baking oven, the reaction time is 4h~for 24 hours；
4th, take out reaction kettle, be cooled to 50 DEG C~70 DEG C, pour out reaction residue, to solid successively with deionized water, diluted acid,
Ethyl alcohol is repeatedly washed, until filtrate is neutrality, 80 DEG C of drying, grinding distribution obtains white powder；
5th, white powder is equably laid in corundum crucible, is put into high temperature furnace and is heat-treated, heating rate is
10 DEG C/min, 1.8-2.0h is kept the temperature again after being raised to set temperature；
6th, after the completion of reacting, crucible is taken out, is cooled to room temperature, ground, encapsulation obtains barium carbonate powder.
In preparation process of the present invention, the best Ba/Ti molar ratios of use are 1.4~1.5, titanium alcohol hybrid mode for ethyl alcohol by
It is added dropwise in butyl titanate.Barium titanium ratio is less than 1.4, and the BT powder crystallinities of synthesis are poor, and higher than 1.5, it is miscellaneous easily to generate other
Matter causes product purity low.
In preparation process of the present invention, ammonium hydroxide is mineralizer, and substance mole is 4~5 times of butyl titanate.Reaction system
The too low synthesis for being unfavorable for BT crystal grain of basicity.
In preparation process of the present invention, 180 DEG C~210 DEG C of the optimal reaction temperature of hydro-thermal reaction, reaction time 20h~for 24 hours.
Reaction time is long and temperature is excessively high, can cause cost excessively high, and the reaction time is insufficient or temperature is too low, is unfavorable for uniformly dividing
The formation of scattered crystal grain.
In preparation process of the present invention, diluted acid can be spirit of vinegar, or dilute formic acid, using sedimentation separation and centrifugation point
From two kinds separation methods.
In preparation process of the present invention, optimum treatment temperature is 1150 DEG C~1200 DEG C.When temperature is higher than 1200 DEG C, easily lead
Powder sintering is caused, during less than 1150 DEG C, content of tetragonal phase is without significant change.
The beneficial effects of the present invention are：
Method of the present invention by the way that hydro-thermal method and heat treatment are combined, has prepared the barium titanate powder of high content of tetragonal phase
Body.Using Ti (C4H9O)4With Ba (OH)2·8H2O is raw material, and asepsis environment-protecting is cheap and easy to get, and ammonium hydroxide is mineralizer, avoids it
The pollution of his alkaline metal ions, ethyl alcohol are solvent, are conducive to the formation of even-grained nanometer-size die, optimum reaction condition
Under, hydrothermal synthesis yield can reach more than 95% theoretical yield, on the barium carbonate powder macroscopic property after 1200 DEG C of heat treatments
Without significant change, tetragonality reaches 1.0091, and Curie temperature is 129 DEG C, and mass loss is only 2.3% before and after heat treatment.This hair
The barium carbonate powder of bright preparation, purity is high, and content of tetragonal phase is high, and manufacturing cost is low, before having important application in MLCC fields
Scape.
Description of the drawings
Fig. 1 is the X-ray diffractogram of the tetra phase barium titanate powder prepared by 1 method of the embodiment of the present invention.
Fig. 2 is the X-ray diffractogram that 2 θ are 44 °~46 ° in Fig. 1.
Fig. 3 is the TEM figures of the barium carbonate powder prepared by 1 method of the embodiment of the present invention.
Specific embodiment
It is further illustrated the present invention with reference to embodiment.
Embodiment 1
Weigh Ba (OH)2·8H2O 11.83g add in 5ml deionized waters in 100ml polytetrafluoroethylliner liners, seal,
It is dissolved by heating under 90 DEG C of water-baths.Weigh Ti (C4H9O)48.51g (Ba/Ti=1.5) in 25ml beakers, is added dropwise under stirring
5ml ethyl alcohol stirs 30min under room temperature.4ml ammonium hydroxide and 5ml deionized waters are uniformly mixed, under stirring state, are added dropwise to
In titanium alcoholic solution, continue to stir 15min after dripping.Titanium precursors are mixed with barium hydroxide solution, reaction kettle compactedness
It is 45%, seal pot is simultaneously put into baking oven, reacts 20h at 210 DEG C.Reaction kettle is taken out, is cooled to 70 DEG C, opens liner, into
Row separation of solid and liquid is repeatedly washed successively with deionized water, spirit of vinegar, ethyl alcohol, until filtrate is neutrality, it is dry at 80 DEG C
For 24 hours, grinding distribution.The barium carbonate powder of preparation is laid in corundum crucible, is put in temperature programming high temperature furnace, at setting heat
It is 1200 DEG C to manage temperature, and heating rate is 10 DEG C/min, and heat preservation 2h postcoolings to room temperature are taken out, and obtain the titanium of high content of tetragonal phase
Sour barium powder, tetragonality c/a values reach 1.0091.Its XRD spectrum is shown in that Fig. 1 and Fig. 2, the TEM of the barium carbonate powder of synthesis shine
Piece is shown in Fig. 3.
Embodiment 2
Weigh Ba (OH)2·8H2O 11.04g add in 5ml deionized waters in 100ml polytetrafluoroethylliner liners, seal,
It is dissolved by heating under 90 DEG C of water-baths.Weigh Ti (C4H9O)48.51g (Ba/Ti=1.4) in 25ml beakers, is added dropwise under stirring
5ml ethyl alcohol stirs 30min under room temperature.4ml ammonium hydroxide and 5ml deionized waters are uniformly mixed, under stirring state, are added dropwise to
In titanium alcoholic solution, continue to stir 15min after dripping.Titanium precursors are mixed with barium hydroxide solution, reaction kettle compactedness
It is 45%, seal pot is simultaneously put into baking oven, is reacted for 24 hours at 180 DEG C.Reaction kettle is taken out, is cooled to 70 DEG C, opens liner, into
Row separation of solid and liquid is repeatedly washed successively with deionized water, dilute formic acid, ethyl alcohol, until filtrate is neutrality, it is dry at 80 DEG C
For 24 hours, grinding distribution.The barium carbonate powder of preparation is laid in corundum crucible, is put in temperature programming high temperature furnace, at setting heat
It is 1150 DEG C to manage temperature, and heating rate is 10 DEG C/min, and heat preservation 2h postcoolings to room temperature are taken out, and obtain the titanium of high content of tetragonal phase
Sour barium powder, tetragonality c/a values reach 1.0092.
Embodiment 3
Weigh Ba (OH)2·8H2O 17.75g add in 5ml deionized waters in 100ml polytetrafluoroethylliner liners, seal,
It is dissolved by heating under 90 DEG C of water-baths.Weigh Ti (C4H9O)412.77g (Ba/Ti=1.5) in 25ml beakers, is added dropwise under stirring
5ml ethyl alcohol stirs 30min under room temperature.6ml ammonium hydroxide and 7.5ml deionized waters are uniformly mixed, under stirring state, are added dropwise
Into titanium alcoholic solution, continue to stir 15min after dripping.Titanium precursors are mixed with barium hydroxide solution, reaction kettle filling
It is 70% to spend, and seal pot is simultaneously put into baking oven, is reacted for 24 hours at 200 DEG C.Reaction kettle is taken out, is cooled to 70 DEG C, opens liner,
Separation of solid and liquid is carried out, is repeatedly washed with deionized water, spirit of vinegar, ethyl alcohol successively, until filtrate is neutrality, it is dry at 80 DEG C
For 24 hours, grinding distribution.The barium carbonate powder of preparation is laid in corundum crucible, is put in temperature programming high temperature furnace, at setting heat
It is 1200 DEG C to manage temperature, and heating rate is 10 DEG C/min, and heat preservation 1.8h postcoolings to room temperature are taken out, and obtain high content of tetragonal phase
Barium carbonate powder, tetragonality c/a values reach 1.0091.
Comparative example 1
Weigh Ba (OH)2·8H2O 10.25g add in 5ml deionized waters in 100ml polytetrafluoroethylliner liners, seal,
It is dissolved by heating under 90 DEG C of water-baths.Weigh Ti (C4H9O)48.51g (Ba/Ti=1.3) in 25ml beakers, is added dropwise under stirring
5ml ethyl alcohol stirs 30min under room temperature.4ml ammonium hydroxide and 5ml deionized waters are uniformly mixed, under stirring state, are added dropwise to
In titanium alcoholic solution, continue to stir 15min after dripping.Titanium precursors are mixed with barium hydroxide solution, reaction kettle compactedness
It is 45%, seal pot is simultaneously put into baking oven, reacts 20h at 210 DEG C.Reaction kettle is taken out, is cooled to 70 DEG C, opens liner, into
Row separation of solid and liquid is repeatedly washed successively with deionized water, spirit of vinegar, ethyl alcohol, until filtrate is neutrality, it is dry at 80 DEG C
For 24 hours, grinding distribution.The barium carbonate powder of preparation is laid in corundum crucible, is put in temperature programming high temperature furnace, at setting heat
It is 1200 DEG C to manage temperature, and heating rate is 10 DEG C/min, and heat preservation 2h postcoolings to room temperature are taken out, and obtain the titanium of high content of tetragonal phase
Sour barium powder, tetragonality c/a values reach 1.0072.
Comparative example 2
Weigh Ba (OH)2·8H2O 11.83g add in 5ml deionized waters in 100ml polytetrafluoroethylliner liners, seal,
It is dissolved by heating under 90 DEG C of water-baths.Weigh Ti (C4H9O)48.51g (Ba/Ti=1.5) in 25ml beakers, is added dropwise under stirring
5ml ethyl alcohol stirs 30min under room temperature.4ml ammonium hydroxide and 5ml deionized waters are uniformly mixed, under stirring state, are added dropwise to
In titanium alcoholic solution, continue to stir 15min after dripping.Titanium precursors are mixed with barium hydroxide solution, reaction kettle compactedness
It is 45%, seal pot is simultaneously put into baking oven, is reacted for 24 hours at 200 DEG C.Reaction kettle is taken out, is cooled to 70 DEG C, opens liner, into
Row separation of solid and liquid is repeatedly washed successively with deionized water, spirit of vinegar, ethyl alcohol, until filtrate is neutrality, it is dry at 80 DEG C
For 24 hours, grinding distribution.The barium carbonate powder of preparation is laid in corundum crucible, is put in temperature programming high temperature furnace, at setting heat
It is 1000 DEG C to manage temperature, and heating rate is 10 DEG C/min, and heat preservation 2h postcoolings to room temperature are taken out, and obtain the titanium of high content of tetragonal phase
Sour barium powder, tetragonality c/a values reach 1.0069.
Claims (7)
1. a kind of preparation method of the barium carbonate powder of high content of tetragonal phase, which is characterized in that include the following steps：
(1) Ti (C are weighed in the ratio that Ba/Ti molar ratios are 1.4~1.54H9O)4With Ba (OH)2·8H2O, by Ti (C4H9O)4With
Ethyl alcohol is mixed by volume for 1: 0.6~1.8 ratio, is stirred 30min under room temperature, is obtained after stirring evenly faint yellow
Prescribed liquid；
(2) take a certain amount of ammonium hydroxide and deionized water, volume ratio 4: 5, after mixing, under agitation, slowly by
It is added drop-wise in above-mentioned transparency liquid, hydrolysis occurs, and leucosol is generated, after ammonium hydroxide dilution drips, in room temperature
Under continue stirring a period of time；
(3) under water bath condition, Ba (OH) is dissolved by heating2·8H2O mixes dissolved barium hydroxide solution with leucosol,
Be fitted into hydrothermal reaction kettle liner, loading be 40%~70%, seal reaction kettle, be put into 100 DEG C~200 DEG C of baking oven into
Row reaction, reaction time 4h~for 24 hours；
(4) reaction kettle is taken out, is cooled to 70 DEG C hereinafter, reaction residue is poured out, to solid successively with deionized water, diluted acid, ethyl alcohol
Repeatedly washing separation is carried out, until filtrate is neutrality, drying, grinding distribution obtains white powder；
(5) white powder is equably laid in corundum crucible, hot place is carried out using the method for temperature programmed control in high temperature furnace
Reason, heating rate are 10 DEG C/min, are raised to after setting heat treatment temperature held for some time again；
(6) after the completion of reacting, crucible is taken out, is cooled to room temperature, the barium carbonate powder of high tetragonality is obtained after grinding.
2. the method for the barium carbonate powder of high content of tetragonal phase is prepared as described in claim 1, which is characterized in that four fourth of metatitanic acid
Ester and ethyl alcohol hybrid mode are added dropwise to for ethyl alcohol in butyl titanate.
3. the method for the barium carbonate powder of high content of tetragonal phase is prepared as described in claim 1, which is characterized in that the step
(2) ammonium hydroxide in is mineralizer, and the wherein molar ratio of ammonia and butyl titanate is 4~5, after ammonium hydroxide dilution is added dropwise to complete, after
Continuous stirring 1-60 minutes.
4. the method for the barium carbonate powder of high content of tetragonal phase is prepared as described in claim 1, which is characterized in that the step
(3) reaction temperature in is 180~210 DEG C, and the reaction time is 20h~for 24 hours.
5. the method for the barium carbonate powder of high content of tetragonal phase is prepared as described in claim 1, which is characterized in that the step
(4) filtering point may be used in mixture of the diluted acid for one or both of spirit of vinegar or dilute formic acid in, the separation method
From or centrifuge two kinds of separation methods.
6. the method for the barium carbonate powder of high content of tetragonal phase is prepared as described in claim 1, which is characterized in that the step
(5) heat treatment temperature is 1150 DEG C~1200 DEG C in, soaking time 1.8-2.0h.
7. the barium carbonate powder of high content of tetragonal phase prepared by the method as described in any one of claim 1-6, tetragonality
(c/a) 1.0090 are all higher than.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109399701A (en) * | 2018-11-16 | 2019-03-01 | 巢湖学院 | A kind of crystal transfer device of hydro-thermal method synthesizing tetragonal barium titanate nano-powder |
| CN110171966A (en) * | 2019-05-30 | 2019-08-27 | 广东三宝新材料科技股份有限公司 | A kind of preparation method of barium titanate-synthetic fluoromica composite material |
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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 |
| CN102531009A (en) * | 2010-12-28 | 2012-07-04 | 上海华明高技术（集团）有限公司 | Nanoscale high-purity aluminum oxide preparation method |
| CN104072128A (en) * | 2014-07-24 | 2014-10-01 | 中国建材国际工程集团有限公司 | Nanoscale square-phase barium titanate powder and preparation method thereof |
| CN105271378A (en) * | 2015-09-29 | 2016-01-27 | 深圳市星源材质科技股份有限公司 | Preparation method of tetragonal barium titanate with high tetragonal rate |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN102531009A (en) * | 2010-12-28 | 2012-07-04 | 上海华明高技术（集团）有限公司 | Nanoscale high-purity aluminum oxide preparation method |
| CN104072128A (en) * | 2014-07-24 | 2014-10-01 | 中国建材国际工程集团有限公司 | Nanoscale square-phase barium titanate powder and preparation method thereof |
| CN105271378A (en) * | 2015-09-29 | 2016-01-27 | 深圳市星源材质科技股份有限公司 | Preparation method of tetragonal barium titanate with high tetragonal rate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109399701A (en) * | 2018-11-16 | 2019-03-01 | 巢湖学院 | A kind of crystal transfer device of hydro-thermal method synthesizing tetragonal barium titanate nano-powder |
| CN109399701B (en) * | 2018-11-16 | 2023-09-12 | 巢湖学院 | Crystal form conversion device for synthesizing tetragonal phase barium titanate nano powder by hydrothermal method |
| CN110171966A (en) * | 2019-05-30 | 2019-08-27 | 广东三宝新材料科技股份有限公司 | A kind of preparation method of barium titanate-synthetic fluoromica composite material |
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