CN105948118B - A kind of porous Bi4Si3O12The preparation method of bulk - Google Patents
A kind of porous Bi4Si3O12The preparation method of bulk Download PDFInfo
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- CN105948118B CN105948118B CN201610292790.4A CN201610292790A CN105948118B CN 105948118 B CN105948118 B CN 105948118B CN 201610292790 A CN201610292790 A CN 201610292790A CN 105948118 B CN105948118 B CN 105948118B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention discloses a kind of porous Bi4Si3O12The preparation method of bulk, using bismuth nitrate and tetraethyl orthosilicate as raw material, mixed solution is solvent, uniform ion is present in xerogel powder using the dispersant of compounding, and porous Bi can be obtained by being molded and being heat-treated through direct pressing4Si3O12Bulk；This method not only make use of the effect of organic matter, make bismuth ion and silicon ion compound evenly, be conducive to the acquisition of pure phase, and effectively shorten manufacturing cycle using one-step method, have the advantages that process equipment is simple and cost is low.
Description
Technical field
The invention belongs to field of material technology, more particularly to a kind of porous Bi4Si3O12The preparation method of bulk.
Background technology
Bismuth oxide has unique conductance, piezoelectricity, photoelectricity, acousto-optic, ferroelectric properties, can be for manufacture electronics pottery
Porcelain, high-selectivity catalyst, phototropic glass, high-temperature superconductor etc., are widely used in Aero-Space, industry, information, biology
The every field such as medical science, Bi2O3-SiO2System is exactly a highly important system in bismuth oxide, and Bi4Si3O12It is
Bi2O3-SiO2Important a kind of stable phase crystal in system.The method for preparing porous material at present mainly uses wet method (such as water
Hot method, colloidal sol-gel method etc.) after synthetic powder material, then the organic matter (such as foaming agent) of compounding is mixed into powder, through system
Porous blocks material is obtained after shaping, heat treatment.Not only the cycle is long for this method, and the distribution of pores in gained porous material is not yet
Enough uniform, for this problem, this patent proposes that a kind of cycle is short, technique is simple and the low one-step preparation method of cost.Using
This method, not only substantially reduces manufacturing cycle, and bismuth ion and silicon ion can be made uniformly to be present in system in favor of
Obtain pure phase Bi4Si3O12。
The content 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 porous Bi4Si3O12Bulk
Preparation method, with simple production process, equipment requirement is simple, the cycle is short the characteristics of.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of porous Bi4Si3O12The preparation method of bulk, comprises the following steps：
(1) dispersant is dissolved in absolute ethyl alcohol and obtains solution A；
(2) measure 1/2 solution A, by tetraethyl orthosilicate be dissolved in wherein formed solution B it is standby；Bismuth nitrate is dissolved in residue
Solution C is formed in solution A；
(3) solution B and solution C are mixed, precursor solution is mixing uniformly to form, by precursor solution in 80~85 DEG C
3~5h is to gelation for lower water-bath, then drying forms xerogel at 140~160 DEG C, is carried out after drying naturally at room temperature ground
Sieve obtains xerogel powder；
(4) it is the dry powder after sieving is directly dry-pressing formed, block blank of material is formed, finally block blank of material is carried out
It is thermally treated resulting in porous Bi4Si3O12Bulk.
In the step (1), the dispersant is by ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, winestone
Acid, ethylene glycol and polyethylene glycol composition.
In the solution A, the concentration range of dispersant each component is 0~0.6mol/L.
The mol ratio that the consumption of the tetraethyl orthosilicate and bismuth oxide meets Si and Bi is (3：4)~(1：1), and Si from
Son is 1 with Bi ions sum and the mol ratio of citric acid：(0.4~0.8).
In the step (4), the heat treatment is to carry out burying burning in ZnO powders, and temperature is 700 DEG C~800 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：The porous Bi that the present invention is provided4Si3O12The preparation of bulk
In method, ethylenediamine tetra-acetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol are rationally utilized
400th, Macrogol 4000, Macrogol 6000 etc. make silicon ion and bismuth ion be uniformly distributed in gel as dispersant, control
All kinds of and consumption of dispersant processed, makes xerogel that the powdered of certain viscosity is presented, xerogel is molded available for direct pressing,
Burnt and appropriate heat treating regime with reference to burying, porous Bi is formed using the foaming and decomposition combustion process of organic matter4Si3O12Block
Material.This method can reduce the preparation process such as granulation, old, make that processing step is few, manufacturing cycle shortens, and utilize
The complexing of machine thing and dispersion effect, make porous Bi4Si3O12Bulk pore-size and distribution controllability are good.
Embodiment
Embodiments of the present invention are described in detail with reference to embodiment.
Embodiment 1
A kind of porous Bi4Si3O12The preparation method of bulk, comprises the following steps：
(1) 50mL absolute ethyl alcohols are measured, a certain amount of dispersant are weighed (by ethylenediamine tetra-acetic acid, citric acid, divinyl three
Amine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol composition, wherein polyethylene glycol include polyethylene glycol 400, polyethylene glycol again
4000 and Macrogol 6000) be added thereto, stirring and dissolving formation solution A, the concentration of dispersant each component is controlled in 0.6mol/
L。
(2) measure 1/2 solution A, by tetraethyl orthosilicate be dissolved in wherein formed solution B it is standby；Bismuth nitrate is dissolved in residue
Solution C is formed in solution A, wherein, Si：Bi (mol ratio)=3：4, (Si ion+Bi ions)：Citric acid (mol ratio)=1：
0.4。
(3) solution B and solution C are mixed, precursor solution is mixing uniformly to form, by precursor solution in water at 80 DEG C
3~5h is bathed to gelation, then drying forms xerogel at 140 DEG C, and powder is ground into sieving after drying naturally at room temperature.
(4) by the direct dry pressing of dry powder after sieving, block blank of material is formed, finally block blank of material exists
Carry out burying burning in ZnO powders, that is, obtain porous Bi4Si3O12Bulk, heat treatment temperature is 800 DEG C.The porous Bi of gained4Si3O12Block
It is open-celled structure in material, crystallite dimension is about 80nm~250nm, and gap size is 50nm~200nm.
Embodiment 2
A kind of porous Bi4Si3O12The preparation method of bulk, comprises the following steps：
(1) 50mL absolute ethyl alcohols are measured, a certain amount of dispersant are weighed (by ethylenediamine tetra-acetic acid, citric acid, divinyl three
Amine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol composition.) be added thereto, stirring and dissolving formation solution A, dispersant each component
Concentration control in 0.6mol/L.
(2) measure 1/2 solution A, by tetraethyl orthosilicate be dissolved in wherein formed solution B it is standby；Bismuth nitrate is dissolved in residue
Solution C is formed in solution A, wherein, Si：Bi (mol ratio)=1：1, (Si ion+Bi ions)：Citric acid (mol ratio)=1：
0.8。
(3) solution B and solution C are mixed, precursor solution is mixing uniformly to form, by precursor solution in water at 85 DEG C
3~5h is bathed to gelation, then drying forms xerogel at 160 DEG C, and powder is ground into sieving after drying naturally at room temperature.
(4) by the direct dry pressing of dry powder after sieving, block blank of material is formed, finally block blank of material exists
Carry out burying to burn in ZnO powders obtaining porous Bi4Si3O12Bulk, heat treatment temperature is 700 DEG C.The porous Bi of gained4Si3O12Block
It is open-celled structure in material, crystallite dimension is about 80nm~250nm, and gap size is 50nm~200nm.
Embodiment 3
A kind of porous Bi4Si3O12The preparation method of bulk, comprises the following steps：
(1) 50mL absolute ethyl alcohols are measured, a certain amount of dispersant are weighed (by ethylenediamine tetra-acetic acid, citric acid, divinyl three
Amine pentacarboxylic acid, tartaric acid, ethylene glycol, polyethylene glycol composition.) be added thereto, stirring and dissolving formation solution A, dispersant each component
Concentration control 0.01,0.1,0.1,0.5,0.5,0.6mol/L.
(2) measure 1/2 solution A, by tetraethyl orthosilicate be dissolved in wherein formed solution B it is standby；Bismuth nitrate is dissolved in residue
Solution C is formed in solution A, wherein, Si：Bi (mol ratio)=3：4, (Si ion+Bi ions)：Citric acid (mol ratio)=1：
0.6。
(3) solution B and solution C are mixed, precursor solution is mixing uniformly to form, by precursor solution in water at 80 DEG C
3~5h is bathed to gelation, then drying forms xerogel at 150 DEG C, and powder is ground into sieving after drying naturally at room temperature.
(4) by the direct dry pressing of dry powder after sieving, block blank of material is formed, finally block blank of material exists
Carry out burying to burn in ZnO powders obtaining porous Bi4Si3O12Bulk, heat treatment temperature is 700 DEG C.The porous Bi of gained4Si3O12Block
It is open-celled structure in material, crystallite dimension is about 80nm~250nm, and gap size is 50nm~200nm.
Claims (3)
1. a kind of porous Bi4Si3O12The preparation method of bulk, it is characterised in that comprise the following steps：
(1) dispersant is dissolved in absolute ethyl alcohol and obtains solution A, the dispersant is by ethylenediamine tetra-acetic acid, citric acid, divinyl
In triamine pentacarboxylic acid, tartaric acid, ethylene glycol and polyethylene glycol composition, solution A, the concentration range of dispersant each component is
0.6mol/L；
(2) measure 1/2 solution A, by tetraethyl orthosilicate be dissolved in wherein formed solution B it is standby；Bismuth nitrate is dissolved in surplus solution A
Middle formation solution C；
(3) solution B and solution C are mixed, precursor solution is mixing uniformly to form, by precursor solution in water at 80~85 DEG C
3~5h is bathed to gelation, then drying forms xerogel at 140~160 DEG C, after drying naturally at room temperature, is ground sieving
Obtain xerogel powder；
(4) it is the dry powder after sieving is directly dry-pressing formed, block blank of material is formed, block blank of material is finally subjected to hot place
Reason obtains porous Bi4Si3O12Bulk.
2. porous Bi according to claim 14Si3O12The preparation method of bulk, it is characterised in that the tetraethyl orthosilicate and
The mol ratio that the consumption of bismuth nitrate meets Si and Bi is (3：4)~(1：, and Si ions and Bi ions sum and citric acid rub 1)
You are than being 1：(0.4~0.8).
3. porous Bi according to claim 14Si3O12The preparation method of bulk, it is characterised in that in the step (4), institute
It is to carry out burying burning in ZnO powders to state heat treatment, and temperature is 700 DEG C~800 DEG C.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821088A (en) * | 2006-03-09 | 2006-08-23 | 上海交通大学 | Process for preparing bismuth silicate nano powder and use |
| CN101157026A (en) * | 2007-11-08 | 2008-04-09 | 北京师范大学 | A preparation method of bismuth silicate powder photocatalyst |
| CN102275942A (en) * | 2011-07-06 | 2011-12-14 | 陕西科技大学 | Preparation method of bismuth silicate nanopowder |
-
2016
- 2016-05-05 CN CN201610292790.4A patent/CN105948118B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1821088A (en) * | 2006-03-09 | 2006-08-23 | 上海交通大学 | Process for preparing bismuth silicate nano powder and use |
| CN101157026A (en) * | 2007-11-08 | 2008-04-09 | 北京师范大学 | A preparation method of bismuth silicate powder photocatalyst |
| CN102275942A (en) * | 2011-07-06 | 2011-12-14 | 陕西科技大学 | Preparation method of bismuth silicate nanopowder |
Non-Patent Citations (3)
| Title |
|---|
| Microwave Dielectric Properties of Sol-Gel Processed;Huidong Xie et al.;《Trans. Ind. Ceram. Soc.》;20150630;第73卷(第2期);第1-3页 * |
| Synthesis of Bi4Si3O12 powders by a sol–gel method;Huidong Xie et al.;《Materials Chemistry and Physics》;20121231;第133卷;第1003-1005页 * |
| 化学溶液分解法制备硅酸铋粉体及其表征;朱常任等;《中国陶瓷》;20100630;第46卷(第6期);第20-22页 * |
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