CN105967747A - Stable-state Bi4Si3O12 porous material preparation method - Google Patents
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- 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
- C04B35/453—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 zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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Abstract
The invention discloses a stable-state Bi4Si3O12 porous material preparation method. The method comprises preparing an ammonia-water solution of citric acid, dissolving bismuth oxide in nitric acid, respectively dissolving the bismuth oxide solution and ethyl orthosilicate through the ammonia-water solution of citric acid, adding dispersants such as ethylene diamine tetraacetic acid, citric acid, diethylenetriaminepentacarboxylic acid, tartaric acid, glycol and polyethylene glycol into the mixed solution, preparing xerogel powder suitable for direct pressing molding and carrying out pressing molding and heat treatment to obtain the stable-state Bi4Si3O12 porous material. The preparation method has the characteristics of simple device, short preparation period and low cost.
Description
Technical field
The invention belongs to field of material technology, particularly to a kind of stable state B i4Si3O12The preparation of porous material
Method.
Background technology
Scintillation crystal Bi4Ge3O12Exist in the application expensive, attenuation constant is higher, photoyield relatively
High problem, and Bi4Si3O12It is then Bi4Ge3O12Best substitute, it is with low-cost SiO2
Substitute expensive GeO2, greatly reduce cost, and and Bi4Ge3O12Compare, its attenuation constant
(100ns) it is only Bi4Ge3O121/3, photoyield is only Bi4Ge3O1220%, and have height
Mechanically and chemically stability and the advantage such as the excellent characteristics of luminescence.Porous ceramics is due to the knot of its porous
Structure, when hole little and when being 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
Increasing, make the most mutually to reunite between nano-particle, nano-particle is the least, then surface activity is the biggest, reunites more
Seriously.If the pore in porous material 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 stable state
Bi4Si3O12The 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 stable state B i4Si3O12The 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 solution A of 1/2, 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;
(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 1~2h 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 stable state B i4Si3O12Porous 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.
It is (4:3)~(1:1) that the consumption of described tetraethyl orthosilicate and bismuth oxide meets the mol ratio of Bi Yu Si,
And the mol ratio of Si ion and Bi ion sum and citric acid is 1:(0.8~1.5).
Described dispersant is by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, second
Glycol and Polyethylene Glycol composition.
After described dispersant adds solution D, in dispersant, the concentration range of each component is 0~0.8mol/L.
The volume of described dehydrated alcohol is the 2/3~1 of ammonia volume.
In described step (4), described heat treatment is to carry out burying burning in ZnO powder body, and temperature is 700 DEG C
~800 DEG C.
Compared with prior art, the invention has the beneficial effects as follows: stable state B i that the present invention provides4Si3O12Many
In the preparation method of Porous materials, with ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, winestone
Acid, ethylene glycol, PEG400, Macrogol 4000, polyethylene glycol 6000 etc. are straight as dispersant
Tap into the gelation process of row complexation foaming, by controlling the concentration of each material, the most each dispersant
Consumption, makes the xerogel of applicable straight forming, and this is possible not only to reduce pelletize, old process,
Crystallization process also can be made to complete with sintering one step.In conjunction with burying the heat treatment process of burning, utilize organic
Bubble and decomposition combustion process form stable state B i4Si3O12Porous material.This method processing step is few, preparation
Cycle is short, equipment is simple, low cost, and gained stable state B i4Si3O12The pore-size of porous material and point
Cloth controllability is good.
Detailed description of the invention
Embodiments of the present invention are described in detail below in conjunction with embodiment.
Embodiment 1
A kind of stable state B i4Si3O12The 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.
(2) measure the solution A of 1/2, 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)=4:3, Si ion
With 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, wherein Polyethylene Glycol include again PEG400,
Macrogol 4000 and polyethylene glycol 6000, the concentration of dispersant each component controls at 0.8mol/L) add
Entering in solution D, (volume of dehydrated alcohol is ammonia volume for addition solution C and absolute ethyl alcohol and stirring dissolving
2/3), afterwards regulation pH value to 1~3 i.e. obtain colloidal sol E.
(4) colloidal sol E water-bath 1~2h 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 stable state B i4Si3O12Porous material, heat treatment temperature
It it is 700 DEG C.Gained stable state B i4Si3O12In porous material, particle size is about 100nm~200nm,
Gap a size of 50nm~180nm.
Embodiment 2
A kind of stable state B i4Si3O12The 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.
(2) measure the solution A of 1/2, 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) 1:1, Si ion
With Bi ion sum: citric acid (mol ratio)=1:1.5.
(3) a certain amount of dispersant is weighed (by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine five carboxylic
Acid, tartaric acid, ethylene glycol, Polyethylene Glycol composition, the concentration of dispersant each component controls at 0.8mol/L.)
Add in solution D, add solution C and absolute ethyl alcohol and stirring dissolves (volume of dehydrated alcohol and ammonia body
Long-pending equal), regulation pH value i.e. obtains colloidal sol E to 1~3 afterwards.
(4) colloidal sol E water-bath 1~2h at 85 DEG C, to gelation, is then dried shape at 160 DEG C
Become 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 stable state B i4Si3O12Porous material, heat treatment temperature
It it is 800 DEG C.Gained stable state B i4Si3O12In porous material, particle size is about 100nm~200nm,
Gap a size of 50nm~180nm.
Embodiment 3
A kind of stable state B i4Si3O12The 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.
(2) measure the solution A of 1/2, 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)=4:3, Si ion
With 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, the concentration of dispersant each component controls 0.01,0.1,
0.1、0.5、0.5、0.8mol/L.) add in solution D, add solution C and absolute ethyl alcohol and stirring is molten
Solving (volume of dehydrated alcohol is the 2/3 of ammonia volume), regulation pH value i.e. obtains molten to 1~3 afterwards
Glue E.
(4) colloidal sol E water-bath 1~2h at 85 DEG C, to gelation, is then dried at 150 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 stable state B i4Si3O12Porous material, heat treatment temperature
It it is 700 DEG C.Gained stable state B i4Si3O12In porous material, particle size is about 100nm~200nm,
Gap a size of 50nm~180nm.
Claims (7)
1. stable state B i4Si3O12The 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 solution A of 1/2, 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;
(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 1~2h 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 stable state B i4Si3O12Porous material.
Stable state B i the most according to claim 14Si3O12The 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.
Stable state B i the most according to claim 14Si3O12The preparation method of porous material, its feature exists
In, it is (4:3)~(1:1) that the consumption of described tetraethyl orthosilicate and bismuth oxide meets the mol ratio of Bi Yu Si,
And the mol ratio of Si ion and Bi ion sum and citric acid is 1:(0.8~1.5).
Stable state B i the most according to claim 14Si3O12The preparation method of porous material, its feature exists
In, described dispersant is by ethylenediaminetetraacetic acid, citric acid, diethylenetriamine pentacarboxylic acid, tartaric acid, second
Glycol and Polyethylene Glycol composition.
Stable state B i the most according to claim 44Si3O12The preparation method of porous material, its feature exists
In, after described dispersant adds solution D, in dispersant, the concentration range of each component is 0~0.8mol/L.
Stable state B i the most according to claim 14Si3O12The preparation method of porous material, its feature exists
In, the volume of described dehydrated alcohol is the 2/3~1 of ammonia volume.
Stable state B i the most according to claim 14Si3O12The 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 700 DEG C
~800 DEG C.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109201035A (en) * | 2018-07-18 | 2019-01-15 | 周口师范学院 | Bi24Ga2O39The preparation method and application of photochemical catalyst |
CN110252350A (en) * | 2019-06-18 | 2019-09-20 | 陕西科技大学 | Bi2O2SiO3/Si2Bi24O40The preparation of/BiOBr double heterojunction composite photo-catalyst |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109201035A (en) * | 2018-07-18 | 2019-01-15 | 周口师范学院 | Bi24Ga2O39The preparation method and application of photochemical catalyst |
CN110252350A (en) * | 2019-06-18 | 2019-09-20 | 陕西科技大学 | Bi2O2SiO3/Si2Bi24O40The preparation of/BiOBr double heterojunction composite photo-catalyst |
CN110252350B (en) * | 2019-06-18 | 2021-09-14 | 陕西科技大学 | Bi2O2SiO3/Si2Bi24O40Preparation of BiOBr double-heterojunction composite photocatalyst |
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Application publication date: 20160928 |