CN105967749A - Preparation method of metastable state Bi2SiO5 porous material - Google Patents
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Abstract
The invention discloses a preparation method of a metastable state Bi2SiO5 porous material. The preparation method comprises preparing an ammonium hydroxide solution of citric acid, dissolving bismuth oxide in nitric acid, respectively dissolving the bismuth oxide solution and ethyl orthosilicate in an ammonium hydroxide solution of citric acid, adding a certain amount of dispersants such as ethylene diamine tetraacetic acid, citric acid, diethylenetriaminepentacarboxylic acid, tartaric acid, glycol and polyethylene glycol into the solution, carrying out gelatinization to prepare xerogel powder suitable for direct pressing molding and carrying out pressing molding and heat treatment to obtain the metastable state Bi2SiO5 porous material. The preparation method has the characteristics of simple processes and equipment, short preparation period and low cost.
Description
Technical field
The invention belongs to field of material technology, particularly to a kind of metastable state Bi2SiO5The system of porous material
Preparation Method.
Background technology
Bi2SiO5It is Bi2O3-SiO2In system, mol ratio is the metastable phase compound of 1: 1, Bi2SiO5
Belonging to the Cmc21 space group of rhombic system, its structure can be regarded as by [Bi2O2]2+It is isolated that layer separates
[SiO3]2-Chain is constituted, and therefore structural formula also can be write as Bi4[O4][Si2O6].Just because of Bi2SiO5Tool
Having above structure, it mainly has the character such as dielectric, thermoelectricity and nonlinear optics, its non-centrosymmetry
Crystal structure also make it possible to that there is ferroelectric property.Porous ceramics, due to the structure of its porous, works as hole
When gap is little and is evenly distributed, the specific surface area of porous ceramics can be made to substantially increase, increased activity.Compared to
Porous nano powder body material, owing to the surface scission of link number of nano-powder material is more, specific surface area increases,
Making the most mutually to reunite between nano-particle, nano-particle is the least, then surface activity is the biggest, reunites the most serious.
If the pore in porous material is evenly distributed, then can solve this problem, and maintain higher ratio table
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 metastable state
Bi2SiO5The preparation method of porous material, has that production technology is simple, equipment requirements is simple, the cycle is short
Feature.
To achieve these goals, the technical solution used in the present invention is:
A kind of metastable state Bi2SiO5The preparation method of porous material, comprises the steps:
(1) citric acid is dissolved in ammonia obtains citric acid solution A, bismuth oxide is dissolved in nitric acid reaction
Form solution B；
(2) measure the citric acid solution A of 1/3, tetraethyl orthosilicate is dissolved in and wherein forms solution C；Will
Solution B is dissolved in residue citric acid solution A and forms solution D；
(3) dispersant is added in solution D, add solution C and absolute ethyl alcohol and stirring is dissolved, it
Rear regulation pH value i.e. obtains colloidal sol E to 1～3；
(4) by colloidal sol E, at 80～85 DEG C, water-bath 1～3h is to gelation, then at 140～160 DEG C
It is dried and forms xerogel, carry out ground sieve after naturally drying under room temperature and obtain xerogel powder body；
(5) dry powder after sieving is the most dry-pressing formed, forms block blank of material, finally by bulk base
Body material carries out being thermally treated resulting in metastable state Bi2SiO5Porous material.
In described step (1), the amount of ammonia is as the criterion can dissolve citric acid, and the amount of nitric acid is with can be the most molten
Solution bismuth oxide is as the criterion.
The consumption of described tetraethyl orthosilicate and bismuth oxide meet the mol ratio of Bi Yu Si for (1:2)～(1:
5), and Si ion and Bi ion sum and the mol ratio of citric acid in step (1) be 1:(0.5～
1.0)。
In described step (2), described dispersant is by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine five
Carboxylic acid, tartaric acid, ethylene glycol and Polyethylene Glycol composition.
After described dispersant adds solution D, the concentration range of dispersant each component is 0～1.0mol/L.
In described step (2), the volume of dehydrated alcohol is the 1/3～1/2 of ammonia volume.
In described step (4), described heat treatment is to carry out burying burning in ZnO powder body, and temperature is 600 DEG C
～700 DEG C.
Compared with prior art, the invention has the beneficial effects as follows: metastable state Bi that the present invention provides2SiO5
In the preparation method of porous material, with ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, wine
Stone acid, ethylene glycol, Polyethylene Glycol (such as PEG400, Macrogol 4000, polyethylene glycol 6000)
Deng directly carrying out the gelation process of complexation foaming as dispersant, by controlling the concentration of each material, special
Not being the consumption of each dispersant, the middle powder body material formed after drying can become bulk material by straight forming,
In this preparation method, bismuth ion and silicon ion is not made to be uniformly present in system merely with dispersant,
Make metastable state Bi2SiO5The crystallization of porous material and recombination process are more uniform, and reduce pelletize, old
Rotten process, makes crystallization process complete with sintering one step, and this all makes manufacturing cycle shorten, and cost reduces.
In conjunction with burying the heat treatment process of burning, organic foaming and decomposition combustion process is utilized to form metastable state
Bi2SiO5Porous material, can obtain metastable state Bi of perforate2SiO5Porous material.
Detailed description of the invention
Embodiments of the present invention are described in detail below in conjunction with embodiment.
Embodiment 1
A kind of metastable state Bi2SiO5The preparation method of porous material, comprises the steps:
(1) citric acid is dissolved in ammonia formation citric acid solution A, and the amount of ammonia is can dissolve citric acid
It is as the criterion；Bismuth oxide being dissolved in nitric acid reaction and forms solution B, nitric acid is as the criterion can be completely dissolved bismuth oxide.
(3) measure the solution A of 1/3, tetraethyl orthosilicate is dissolved in and wherein forms solution C；By solution B
It is dissolved in residue citric acid solution and forms solution D, wherein, Bi:Si (mol ratio)=1:2, Si ion
With Bi ion sum: citric acid (mol ratio)=1:0.5.
(3) a certain amount of dispersant is weighed (by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine five carboxylic
Acid, tartaric acid, ethylene glycol, Polyethylene Glycol composition, wherein Polyethylene Glycol include again PEG400,
Macrogol 4000 and polyethylene glycol 6000.) add in solution D, the concentration control of dispersant each component
Making at 1.0mol/L, (volume of dehydrated alcohol is ammonia body for addition solution C and absolute ethyl alcohol and stirring dissolving
Long-pending 1/3), regulation pH value i.e. obtains colloidal sol E to 1～3 afterwards.
(4) colloidal sol E water-bath 1～3h at 80 DEG C, to gelation, is then dried at 140 DEG C and is formed
Xerogel, by powder body is ground sieve after naturally drying under room temperature.
(5) the direct dry pressing of dry powder after sieving, forms block blank of material, finally by bulk base
Body material carries out burying burning in ZnO powder body and i.e. obtains metastable state Bi2SiO5Porous material, heat treatment temperature
It it is 600 DEG C.Gained metastable state Bi2SiO5Being open-celled structure in porous material, crystallite dimension is about 150
Nm～500nm, gap size is 80nm～200nm.
Embodiment 2
A kind of metastable state Bi2SiO5The preparation method of porous material, comprises the steps:
(1) citric acid is dissolved in ammonia formation citric acid solution A, and the amount of ammonia is can dissolve citric acid
It is as the criterion；Bismuth oxide being dissolved in nitric acid reaction and forms solution B, nitric acid is as the criterion can be completely dissolved bismuth oxide.
(3) measure the solution A of 1/3, tetraethyl orthosilicate is dissolved in and wherein forms solution C；By solution B
It is dissolved in residue citric acid solution and forms solution D, wherein, the ratio of Bi:Si (mol ratio)=1:5,
Si ion and Bi ion sum: citric acid (mol ratio)=1:1.
(3) a certain amount of dispersant is weighed (by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine five carboxylic
Acid, tartaric acid, ethylene glycol, Polyethylene Glycol composition.) add in solution D, dispersant each component dense
Degree controls at 1.0mol/L, and (volume of dehydrated alcohol is ammonia for addition solution C and absolute ethyl alcohol and stirring dissolving
The 1/2 of water volume), regulation pH value i.e. obtains colloidal sol E to 1～3 afterwards.
(4) colloidal sol E water-bath 1～3h at 85 DEG C, to gelation, is then dried at 140 DEG C and is formed
Xerogel, by powder body is ground sieve after naturally drying under room temperature.
(5) the direct dry pressing of dry powder after sieving, forms block blank of material, finally by bulk base
Body material carries out burying burning in ZnO powder body and i.e. obtains metastable state Bi2SiO5Porous material, heat treatment temperature
It it is 700 DEG C.Gained metastable state Bi2SiO5Being open-celled structure in porous material, crystallite dimension is about 150
Nm～500nm, gap size is 80nm～200nm.
Embodiment 3
A kind of metastable state Bi2SiO5The preparation method of porous material, comprises the steps:
(1) citric acid is dissolved in ammonia formation citric acid solution A, and the amount of ammonia is can dissolve citric acid
It is as the criterion；Bismuth oxide being dissolved in nitric acid reaction and forms solution B, nitric acid is as the criterion can be completely dissolved bismuth oxide.
(3) measure the solution A of 1/3, tetraethyl orthosilicate is dissolved in and wherein forms solution C；By solution B
It is dissolved in residue citric acid solution and forms solution D, wherein, the ratio of Bi:Si (mol ratio)=1:3,
Si ion and Bi ion sum: citric acid (mol ratio)=1:0.8.
(3) a certain amount of dispersant is weighed (by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine five carboxylic
Acid, tartaric acid, ethylene glycol, Polyethylene Glycol composition.) add in solution D, dispersant each component dense
Degree controls 0.01,0.1,0.1,0.5,0.5,1.0mol/L, add solution C and absolute ethyl alcohol and stirring
Dissolving (volume of dehydrated alcohol is the 1/2 of ammonia volume), regulation pH value i.e. obtains to 1～3 afterwards
Colloidal sol E.
(4) by colloidal sol E at 80 DEG C～85 DEG C water-bath 1～3h to gelation, then at 140 DEG C～
It is dried at 160 DEG C and forms xerogel, be ground sieving by powder body after naturally drying under room temperature.
(5) the direct dry pressing of dry powder after sieving, forms block blank of material, finally by bulk base
Body material carries out burying burning in ZnO powder body and i.e. obtains metastable state Bi2SiO5Porous material, heat treatment temperature
It it is 600 DEG C.Gained metastable state Bi2SiO5Being open-celled structure in porous material, crystallite dimension is about 150
Nm～500nm, gap size is 80nm～200nm.
Claims (7)
1. metastable state Bi2SiO5The preparation method of porous material, it is characterised in that include walking as follows
Rapid:
(1) citric acid is dissolved in ammonia obtains citric acid solution A, bismuth oxide is dissolved in nitric acid reaction
Form solution B；
(2) measure the citric acid solution A of 1/3, tetraethyl orthosilicate is dissolved in and wherein forms solution C；Will
Solution B is dissolved in residue citric acid solution A and forms solution D；
(3) dispersant is added in solution D, add solution C and absolute ethyl alcohol and stirring is dissolved, it
Rear regulation pH value i.e. obtains colloidal sol E to 1～3；
(4) by colloidal sol E, at 80～85 DEG C, water-bath 1～3h is to gelation, then at 140～160 DEG C
It is dried and forms xerogel, carry out ground sieve after naturally drying under room temperature and obtain xerogel powder body；
(5) dry powder after sieving is the most dry-pressing formed, forms block blank of material, finally by bulk base
Body material carries out being thermally treated resulting in metastable state Bi2SiO5Porous material.
Metastable state Bi the most according to claim 12SiO5The preparation method of porous material, its feature exists
In, in described step (1), the amount of ammonia is as the criterion can dissolve citric acid, and the amount of nitric acid is with can be the most molten
Solution bismuth oxide is as the criterion.
Metastable state Bi the most according to claim 12SiO5The preparation method of porous material, its feature exists
In, the consumption of described tetraethyl orthosilicate and bismuth oxide meet the mol ratio of Bi Yu Si for (1:2)～(1:
5), and Si ion and Bi ion sum and the mol ratio of citric acid in step (1) be 1:(0.5～
1.0)。
Metastable state Bi the most according to claim 12SiO5The preparation method of porous material, its feature exists
In, in described step (2), described dispersant is by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine five
Carboxylic acid, tartaric acid, ethylene glycol and Polyethylene Glycol composition.
Metastable state Bi the most according to claim 42SiO5The preparation method of porous material, its feature exists
In, after described dispersant adds solution D, the concentration range of dispersant each component is 0～1.0mol/L.
Metastable state Bi the most according to claim 42SiO5The preparation method of porous material, its feature exists
In, in described step (2), the volume of dehydrated alcohol is the 1/3～1/2 of ammonia volume.
Metastable state Bi the most according to claim 12SiO5The preparation method of porous material, its feature exists
In, in described step (4), described heat treatment is to carry out burying burning in ZnO powder body, and temperature is 600 DEG C
～700 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110252341A (en) * | 2019-06-18 | 2019-09-20 | 陕西科技大学 | A kind of Bi2O2SiO3/Bi2O3The preparation method of/BiOBr Heterogeneous Composite luminescent material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110252341A (en) * | 2019-06-18 | 2019-09-20 | 陕西科技大学 | A kind of Bi2O2SiO3/Bi2O3The preparation method of/BiOBr Heterogeneous Composite luminescent material |
| CN110252341B (en) * | 2019-06-18 | 2021-11-16 | 陕西科技大学 | Bi2O2SiO3/Bi2O3Preparation method of BiOBr heterogeneous composite light material |
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Application publication date: 20160928 |