CN105967748A - Preparation method of BaTiO3 porous material - Google Patents

Preparation method of BaTiO3 porous material Download PDF

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CN105967748A
CN105967748A CN201610292780.0A CN201610292780A CN105967748A CN 105967748 A CN105967748 A CN 105967748A CN 201610292780 A CN201610292780 A CN 201610292780A CN 105967748 A CN105967748 A CN 105967748A
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preparation
citric acid
solution
batio
porous ceramics
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伍媛婷
栗梦龙
王秀峰
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • 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
    • C04B35/4682—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 based on BaTiO3 perovskite phase
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C04B35/634—Polymers
    • C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • C04B38/0058—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity open porosity
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Abstract

The invention discloses a preparation method of a BaTiO3 porous material. The preparation method comprises dissolving citric acid in ammonium hydroxide, dissolving bismuth oxide in nitric acid, respectively dissolving the bismuth oxide solution and ethyl orthosilicate in an ammonium hydroxide solution of citric acid, adding dispersants such as ethylene diamine tetraacetic acid, citric acid, diethylenetriaminepentacarboxylic acid, tartaric acid, glycol and polyethylene glycol into the solution, preparing xerogel powder suitable for direct pressing molding and carrying out pressing molding and heat treatment to obtain a BaTiO3 porous ceramic. The preparation method has the characteristics of simple processes and equipment, short preparation period and low cost.

Description

A kind of BaTiO3The preparation method of porous ceramics
Technical field
The invention belongs to field of material technology, particularly to a kind of BaTiO3The preparation method of porous ceramics.
Background technology
Barium metatitanate. (BaTiO3) belong to typical perovskite (ABO3) structure, there is the piezoelectricity ferrum of excellence Electrically, high dielectric constant and high positive temperature coefficient etc., be a kind of important ceramic material.Metatitanic acid Barium porous ceramics due to the structure of its porous, when hole little and when being evenly distributed, Barium metatitanate. porous can be made to make pottery The specific surface area of porcelain substantially increases, increased activity.Compared to porous nano barium carbonate powder material, due to The surface scission of link number of nano-powder material is more, and specific surface area increases, and makes easy phase between barium titanate nano granule Reuniting mutually, nano-particle is the least, then surface activity is the biggest, reunites the most serious.If Barium metatitanate. porous is made pottery Pore in porcelain is evenly distributed, then can solve this problem, and maintain higher specific surface area and surface Activity.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, it is an object of the invention to provide a kind of BaTiO3Porous The preparation method of pottery, has the advantages that production technology is simple, equipment requirements is simple, the cycle is short.
To achieve these goals, the technical solution used in the present invention is:
A kind of BaTiO3The preparation method of porous ceramics, comprises the steps:
(1) citric acid is dissolved in ammonia obtains citric acid solution, measure the citric acid solution of 1/2, will Barium acetate is dissolved in wherein, forms solution A standby；Butyl titanate is dissolved in residue citric acid solution and being formed Solution B；
(2) solution A and solution B are mixed, be stirring evenly and then adding into dispersant, add anhydrous second Alcohol stirring and dissolving, regulation pH value obtains colloidal sol C to 5～7 afterwards；
(3) by colloidal sol C, at 80～85 DEG C, water-bath 2～4h is to gelation, then at 140～160 DEG C Being dried and form xerogel, after drying 1h at 200 DEG C～250 DEG C, natural cooling, being ground sieving obtains Xerogel powder body；
(4) by the most dry-pressing formed for xerogel powder body, block blank of material is formed, finally by bulk base substrate Material carries out being thermally treated resulting in BaTiO3Porous ceramics.
In described step (1), the amount of ammonia is as the criterion can dissolve citric acid.
It is 1:1 that the consumption of described barium nitrate and butyl titanate meets the mol ratio of Ba Yu Ti, and Ba ion It is 1:(1～2 with the mol ratio of Ti ion sum Yu citric acid).
Described dispersant is by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, second Glycol and Polyethylene Glycol composition.
After adding dispersant in described solution A and solution B, the concentration range of dispersant each component is 0～0.8mol/L.
The volume of described dehydrated alcohol is 1～2 times of ammonia volume.
In described step (4), described heat treatment be in ZnO powder body 700 DEG C bury burning 1h, then 1～3h is sintered at 1000～1400 DEG C.
Compared with prior art, the invention has the beneficial effects as follows: the BaTiO that the present invention provides3Porous ceramics Preparation method in, with ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, second The conducts such as glycol, Polyethylene Glycol (such as PEG400, Macrogol 4000, polyethylene glycol 6000) Dispersant directly carries out the gelation process of complexation foaming, by controlling the concentration of each material, respectively The consumption of dispersant, the middle powder body material formed after drying can become bulk material by straight forming, at this In individual preparation method, do not make titanium ion and barium ions be uniformly present in system merely with dispersant, make BaTiO3The crystallization process of porous ceramics is more uniform, and reduces pelletize, old process, makes crystallization Process completes with sintering one step, and this all makes manufacturing cycle shorten, and cost reduces.In conjunction with the heat treatment burying burning Process, utilizes organic foaming and decomposition combustion process to form BaTiO3Porous ceramics, can obtain perforate Structure.
Detailed description of the invention
Embodiments of the present invention are described in detail below in conjunction with embodiment.
Embodiment 1
A kind of BaTiO3The preparation method of porous ceramics, comprises the steps:
(1) being dissolved in by citric acid in ammonia (volumetric concentration 25%～28%), the amount of ammonia is dissolving Citric acid is as the criterion, and measures the citric acid solution of 1/2, barium acetate is dissolved in wherein formation solution A standby； Being dissolved in by butyl titanate in residue citric acid solution and form solution B, wherein, Ba:Ti (mol ratio) accords with Close stoichiometric proportion 1:1, and the mol ratio of Ba ion and Ti ion sum and citric acid is=1:1.
(2) mixed solution A and solution B, weighs a certain amount of dispersant (by second two after stirring Amine tetraacethyl, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol, Polyethylene Glycol form, Wherein Polyethylene Glycol includes again PEG400, Macrogol 4000 and polyethylene glycol 6000) add it In, the concentration of dispersant each component controls at 0.8mol/L, adds absolute ethyl alcohol and stirring and dissolves (anhydrous The volume of ethanol is 2 times of ammonia volume), regulation pH value to 5～7 i.e. obtains colloidal sol C.
(3) by colloidal sol C at 80 DEG C water-bath 2～4h to gelation.It is dried to be formed at 140 DEG C again and does Gel, after drying 1h at 200 DEG C, natural cooling, it is ground sieving by powder body.
(4) the direct dry pressing of dry powder after sieving, forms block blank of material, finally by bulk base Body material in ZnO powder body 700 DEG C carry out burying burning 1h, at 1000 DEG C, sinter 1h more i.e. obtain BaTiO3Porous material.Gained BaTiO3Being open-celled structure in porous material, crystallite dimension is about 150 Nm～300nm, gap size is 100nm～200nm.
Embodiment 2
A kind of BaTiO3The preparation method of porous ceramics, comprises the steps:
(1) being dissolved in by citric acid in ammonia (volumetric concentration 25%～28%), the amount of ammonia is dissolving Citric acid is as the criterion, and measures the citric acid solution of 1/2, barium acetate is dissolved in wherein formation solution A standby； Being dissolved in by butyl titanate in residue citric acid solution and form solution B, wherein, Ba:Ti (mol ratio) accords with Close stoichiometric proportion 1:1, and the mol ratio of Ba ion and Ti ion sum and citric acid is=1:2.
(2) mixed solution A and solution B, weighs a certain amount of dispersant (by second two after stirring Amine tetraacethyl, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol, Polyethylene Glycol form) Being added thereto, the concentration of dispersant each component controls at 0.8mol/L, adds absolute ethyl alcohol and stirring and dissolves (volume of dehydrated alcohol is equal with ammonia volume), regulation pH value to 5～7 i.e. obtains colloidal sol C.
(3) by colloidal sol C at 85 DEG C water-bath 2～4h to gelation.It is dried to be formed at 160 DEG C again and does Gel, after drying 1h at 250 DEG C, natural cooling, it is ground sieving by powder body.
(4) the direct dry pressing of dry powder after sieving, forms block blank of material, finally by bulk base Body material in ZnO powder body 700 DEG C carry out burying burning 1h, at 1400 DEG C, sinter 1h more i.e. obtain BaTiO3Porous material.Gained BaTiO3Being open-celled structure in porous material, crystallite dimension is about 150 Nm～300nm, gap size is 100nm～200nm.
Embodiment 3
A kind of BaTiO3The preparation method of porous ceramics, comprises the steps:
(1) being dissolved in by citric acid in ammonia (volumetric concentration 25%～28%), the amount of ammonia is dissolving Citric acid is as the criterion, and measures the citric acid solution of 1/2, barium acetate is dissolved in wherein formation solution A standby； Being dissolved in by butyl titanate in residue citric acid solution and form solution B, wherein, Ba:Ti (mol ratio) accords with Close stoichiometric proportion 1:1, and the mol ratio of Ba ion and Ti ion sum and citric acid is=1:1.5.
(2) mixed solution A and solution B, weighs a certain amount of dispersant (by second two after stirring Amine tetraacethyl, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol, Polyethylene Glycol form) Be added thereto, the concentration of dispersant each component controls 0.01,0.1,0.1,0.5,0.7,0.8mol/L, Add absolute ethyl alcohol and stirring and dissolve 2 times of ammonia volume (volume of dehydrated alcohol be), regulate pH It is worth to 5～7 and i.e. obtains colloidal sol C.
(3) by colloidal sol C at 80 DEG C water-bath 2～4h to gelation.It is dried to be formed at 150 DEG C again and does Gel, after drying 1h at 220 DEG C, natural cooling, it is ground sieving by powder body.
(4) the direct dry pressing of dry powder after sieving, forms block blank of material, finally by bulk base Body material in ZnO powder body 700 DEG C carry out burying burning 1h, at 1200 DEG C, sinter 2h more i.e. obtain BaTiO3Porous material.Gained BaTiO3Being open-celled structure in porous material, crystallite dimension is about 150 Nm～300nm, gap size is 100nm～200nm.

Claims (7)

1. a BaTiO3The preparation method of porous ceramics, it is characterised in that comprise the steps:
(1) citric acid is dissolved in ammonia obtains citric acid solution, measure the citric acid solution of 1/2, will It is standby that barium acetate is dissolved in wherein formation solution A；Butyl titanate is dissolved in residue citric acid solution in formed molten Liquid B；
(2) solution A and solution B are mixed, be stirring evenly and then adding into dispersant, add anhydrous second Alcohol stirring and dissolving, regulation pH value obtains colloidal sol C to 5～7 afterwards；
(3) by colloidal sol C, at 80～85 DEG C, water-bath 2～4h is to gelation, then at 140～160 DEG C Being dried and form xerogel, after drying 1h at 200 DEG C～250 DEG C, natural cooling, being ground sieving obtains Xerogel powder body；
(4) by the most dry-pressing formed for xerogel powder body, block blank of material is formed, finally by bulk base substrate Material carries out being thermally treated resulting in BaTiO3Porous ceramics.
BaTiO the most according to claim 13The preparation method of porous ceramics, it is characterised in that institute Stating in step (1), the amount of ammonia is as the criterion can dissolve citric acid.
BaTiO the most according to claim 13The preparation method of porous ceramics, it is characterised in that institute State the consumption of barium nitrate and butyl titanate meeting the mol ratio of Ba Yu Ti is 1:1, and Ba ion and Ti Ion sum is 1:(1～2 with the mol ratio of citric acid).
BaTiO the most according to claim 13The preparation method of porous ceramics, it is characterised in that institute State dispersant by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol and Polyethylene Glycol forms.
BaTiO the most according to claim 43The preparation method of porous ceramics, it is characterised in that institute Stating after adding dispersant in solution A and solution B, the concentration range of dispersant each component is 0～0.8mol/L.
BaTiO the most according to claim 13The preparation method of porous ceramics, it is characterised in that institute The volume stating dehydrated alcohol is 1～2 times of ammonia volume.
BaTiO the most according to claim 13The preparation method of porous ceramics, it is characterised in that institute State in step (4), described heat treatment be in ZnO powder body 700 DEG C bury burning 1h, then at 1000～1400 DEG C Lower sintering 1～3h.
CN201610292780.0A 2016-05-05 2016-05-05 Preparation method of BaTiO3 porous material Pending CN105967748A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1796552A (en) * 2004-12-29 2006-07-05 华东理工大学 Method for preparing porous material in lumpy in use for biological zymophore
CN101602521A (en) * 2009-07-15 2009-12-16 中山大学 A kind of porous BaTiO 3The synthetic method of nano particle balls
CN101891466A (en) * 2010-07-21 2010-11-24 陕西科技大学 Method for preparing tabular barium titanate nanometer powder
CN102584215A (en) * 2011-12-14 2012-07-18 浙江理工大学 Method for preparing classified porous tetragonal-phase barium titanate ceramics materials

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1796552A (en) * 2004-12-29 2006-07-05 华东理工大学 Method for preparing porous material in lumpy in use for biological zymophore
CN101602521A (en) * 2009-07-15 2009-12-16 中山大学 A kind of porous BaTiO 3The synthetic method of nano particle balls
CN101891466A (en) * 2010-07-21 2010-11-24 陕西科技大学 Method for preparing tabular barium titanate nanometer powder
CN102584215A (en) * 2011-12-14 2012-07-18 浙江理工大学 Method for preparing classified porous tetragonal-phase barium titanate ceramics materials

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
米晓云 等: "《Al2O3纳米粉体及透明陶瓷》", 31 March 2012, 吉林大学出版社 *
衣宝廉: "《燃料电池—原理·技术·应用》", 31 August 2003, 化学工业出版社 *

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Application publication date: 20160928