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 PDF

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Publication number
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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barium carbonate
carbonate powder
tetragonal phase
powder
high content
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程鏖
李婷
孔凡滔
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Shanghai Huaming Hi Tech Group Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/46Shaped 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
    • C04B35/462Shaped 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
    • C04B35/465Shaped 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
    • C04B35/468Shaped 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
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
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  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

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

A kind of low temperature preparation method of electronic ceramics powder
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.
CN201611173805.1A 2016-12-16 2016-12-16 A kind of low temperature preparation method of electronic ceramics powder Pending CN108203298A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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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Publication number Priority date Publication date Assignee Title
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
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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