CN104192854A - Method for preparing bismuth silicate powder - Google Patents
Method for preparing bismuth silicate powder Download PDFInfo
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- CN104192854A CN104192854A CN201410317866.5A CN201410317866A CN104192854A CN 104192854 A CN104192854 A CN 104192854A CN 201410317866 A CN201410317866 A CN 201410317866A CN 104192854 A CN104192854 A CN 104192854A
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- sodium silicate
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Abstract
The invention provides a method for preparing bismuth silicate powder. The method comprises the following steps: weighing bismuth salt, sodium silicate and a reducing agent which are in a molar ratio of (1-12) to (1-2) to (10-30); dissolving the sodium silicate in deionized water to obtain a sodium silicate solution with the concentration between 0.5mol/L and 2mol/L; completely dissolving the reducing agent in deionized water to obtain a reducing agent solution; and completely dissolving the bismuth salt in deionized water or a nitric acid solution, then pouring the sodium silicate solution and the reducing agent solution into the solution, heating to 80 DEG C to 100 DEG C by virtue of a magnetic stirrer, continuously stirring, transferring the mixed solution into a high-temperature sintering furnace which is preheated to 600 DEG C to 800 DEG C, and severely burning along with the evaporation of water so as to obtain a fluffy foam-shaped product. The method carried out by taking the sodium silicate with a relatively low cost as a raw material is available for practical applications; and the prepared powder is good in dispersibility and thin and small in granules. In addition, the method requires simple equipment and is simple in process.
Description
Technical field
The invention belongs to inorganic non-metallic ultrafine powder field, relate in particular to a kind of bismuth silicate powder, specifically a kind of method of preparing bismuth silicate powder.
Background technology
Different according to the content of bismuth in compound and silicon, bismuth silicate is mainly divided into two classes, the one, Bi
4si
3o
12, the one, Bi
12siO
20.The former is a kind of important scintillation crystal, it and the bismuth germanium oxide (Bi being widely used at present
4ge
3o
12bGO) have similar physicochemical property, its decay of afterglow is faster than BGO, and Radiation Hardness is larger than BGO, particularly the low cost of BSO becomes the ideal material that substitutes BGO, is applied in the fields such as nuclear physics, high energy physics, nuclear medicine, safety inspection.The latter is a kind of multifunctional light information material, it be have that electricity, photoconduction, light are sold off simultaneously, the non-ferroelectric cubic oxide thing crystal of piezoelectricity and the effect such as opticity and Faraday optically-active, have a wide range of applications at aspects such as light amplification, phase conjugate compensation, Hologram Storage, image processing and surface acoustic wave devices.
Obtain high-quality crystalline material or transparent ceramic material, raw material is primarily to solve key factor.At present mainly obtain bismuth silicate powder by high temperature solid state reaction and sol-gel method, but high temperature solid-state method sintering temperature is higher, long reaction time, the product particle of acquisition is thicker, and the follow-up pulverizing process of needs could be levigate by product.Sol-gel method is a kind of emerging wet chemical synthesis, although the powder making can reach nano level, operation is loaded down with trivial details, wayward, and alkoxide used is not only expensive, and is harmfully unfavorable for scale operation.
Summary of the invention
For above-mentioned the problems referred to above of the prior art, the invention provides a kind of method of preparing bismuth silicate powder, it is not only expensive that the described this method of preparing bismuth silicate powder will solve loaded down with trivial details, the wayward and used alkoxide of preparation method's operation of the prior art, and harmful technical problem.
A kind of method of preparing bismuth silicate powder of the present invention, comprises the following steps:
1) take bismuth salt, water glass, reductive agent, the mol ratio of described bismuth salt, water glass, reductive agent is 1 ~ 12:1 ~ 2:10 ~ 30;
2) water glass is dissolved in deionized water and obtains sodium silicate solution, the concentration of described sodium silicate solution is between 0.5 ~ 2mol/L;
3) reductive agent is dissolved in deionized water completely, obtains reductant solution;
4) bismuth salt is dissolved in deionized water or salpeter solution completely, again sodium silicate solution and reductant solution are poured into, be heated to subsequently 80 ~ 100 DEG C, continue to stir after 3 ~ 10 minutes, direct solution immigration is heated in advance in the high temperature sintering furnace of 600 ~ 800 DEG C, along with the evaporation of moisture, obtain bismuth silicate powder.
Further, described bismuth salt is any one in Bismuth trinitrate, Bismuth carbonate.
Further, described reductive agent is any one in urea, citric acid, L-glutamic acid.
Further, the concentration of described salpeter solution is between 0.5 ~ 2mol/L.
The present invention replaces tetraethoxy as raw material and adopts combustion synthesis technology to prepare taking sodium silicate solution, thereby does not have the problems such as sol-gel method raw material costliness, technique are loaded down with trivial details, thereby has with low cost, the simple technique effect of technique.
The present invention does not need external heat source long duration of action, does not therefore have the problems such as sintering temperature is higher, long reaction time, thereby few technique effect that has that thermal treatment temp is low, quick, product is reunited.
The present invention has adopted combustion synthesis method, thereby does not exist solid state sintering to need external heat source and the problem such as sol-gel method technique is loaded down with trivial details, thereby it is high to have efficiency, is conducive to reduce manufacturing cost, is easy to the technique effect of industrialization.
The present invention compares with prior art, and its technical progress is significant.It is raw material that the present invention adopts the relatively inexpensive water glass of cost, is conducive to practical application; The powder good dispersion making, particle is tiny; Equipment, technique are simple.
Brief description of the drawings
Fig. 1 is the XRD figure spectrum of embodiment 1;
Fig. 2 is the SEM electromicroscopic photograph of embodiment 1.
Embodiment
Below by specific embodiment, also the present invention is further elaborated by reference to the accompanying drawings, but do not limit the present invention.
Embodiment 1
In Bismuth trinitrate: water glass: urea=4:3:15 ratio batching, water glass is dissolved in deionized water and obtains sodium silicate solution, the concentration of silicon sodium solution is at 0.5mol/L, and urea is dissolved in deionized water completely.Bismuth trinitrate is dissolved in deionized water completely, again sodium silicate solution and urea soln are poured into, be heated to 80 DEG C with magnetic stirring apparatus subsequently, continue to stir after 3 minutes, direct solution immigration is heated in advance in the high temperature sintering furnace of 750 DEG C, along with the evaporation of moisture, violent burning, obtains fluffy spumescence product, and its XRD and SEM figure are respectively as depicted in figs. 1 and 2, from XRD figure, product is bismuth silicate (Bi substantially
4si
3o
12) phase, from SEM figure, can find out, the median size of silicic acid bismuth meal is 0.25 μ m.
Embodiment 2
In Bismuth trinitrate: water glass: urea=4:3:26 ratio batching, water glass is dissolved in deionized water and obtains sodium silicate solution, the concentration of sodium silicate solution is at 1.5mol/L, and urea is dissolved in deionized water completely.Bismuth trinitrate is dissolved in deionized water completely, again sodium silicate solution and urea soln are poured into, be heated to 100 DEG C with magnetic stirring apparatus subsequently, continue to stir after 5 minutes, direct solution immigration is heated in advance in the high temperature sintering furnace of 600 DEG C, all the other implementation conditions are all with embodiment 1, have obtained the bismuth silicate (Bi that median size is about 0.18 μ m
4si
3o
12) powder.
Embodiment 3
In bismuth hydroxide: water glass: urea=4:3:10 ratio batching, water glass is dissolved in deionized water and obtains sodium silicate solution, the concentration of sodium silicate solution is at 0.5mol/L, and urea is dissolved in deionized water completely.Bismuth hydroxide is dissolved in nitric acid completely, again sodium silicate solution and urea soln are poured into, be heated to 100 DEG C with magnetic stirring apparatus subsequently, continue to stir after 10 minutes, direct solution immigration is heated in advance in the high temperature sintering furnace of 800 DEG C, all the other implementation conditions are all with embodiment 1, have obtained the bismuth silicate (Bi that median size is about 0.32 μ m
4si
3o
12) powder.
Embodiment 4
In Bismuth carbonate: water glass: urea=4:3:28 ratio batching, water glass is dissolved in deionized water and obtains sodium silicate solution, the concentration of sodium silicate solution is at 0.5mol/L, and urea is dissolved in deionized water completely.Bismuth carbonate is dissolved in nitric acid completely, again sodium silicate solution and urea soln are poured into, be heated to 100 DEG C with magnetic stirring apparatus subsequently, continue to stir after 3 minutes, direct solution immigration is heated in advance in the high temperature sintering furnace of 800 DEG C, all the other implementation conditions are all with embodiment 1, have obtained the bismuth silicate (Bi that median size is about 0.24 μ m
4si
3o
12) powder.
Embodiment 5
In Bismuth trinitrate: water glass: urea=12:1:30 ratio batching, water glass is dissolved in deionized water and obtains sodium silicate solution, the concentration of sodium silicate solution is at 1.5mol/L, and urea is dissolved in deionized water completely.Bismuth carbonate is dissolved in nitric acid completely, again sodium silicate solution and urea soln are poured into, be heated to 100 DEG C with magnetic stirring apparatus subsequently, continue to stir after 3 minutes, direct solution immigration is heated in advance in the high temperature sintering furnace of 800 DEG C, all the other implementation conditions are all with embodiment 1, have obtained the calcium magnesium silicate (Bi that median size is about 0.28 μ m
12siO
20) powder.
Embodiment 6
In Bismuth trinitrate: water glass: citric acid=4:3:4 ratio batching, water glass is dissolved in deionized water and obtains sodium silicate solution, the concentration of sodium silicate solution is at 0.5mol/L, and citric acid is dissolved in deionized water completely.Bismuth trinitrate is dissolved in deionized water completely, again sodium silicate solution and citric acid solution are poured into, be heated to 100 DEG C with magnetic stirring apparatus subsequently, continue to stir after 3 minutes, direct solution immigration is heated in advance in the high temperature sintering furnace of 800 DEG C, all the other implementation conditions are all with embodiment 1, have obtained the calcium magnesium silicate (Bi that median size is about 0.24 μ m
4si
3o
20) powder.
Embodiment 7
In Bismuth trinitrate: water glass: L-glutamic acid=4:3:26 ratio batching, water glass is dissolved in deionized water and obtains sodium silicate solution, the concentration of sodium silicate solution is at 0.5mol/L, and L-glutamic acid is dissolved in deionized water completely.Bismuth trinitrate is dissolved in deionized water completely, again sodium silicate solution and glutamic acid solution are poured into, be heated to 80 DEG C with magnetic stirring apparatus subsequently, continue to stir after 3 minutes, direct solution immigration is heated in advance in the high temperature sintering furnace of 700 DEG C, all the other implementation conditions are all with embodiment 1, have obtained the calcium magnesium silicate (Bi that median size is about 0.26 μ m
4si
3o
12) powder.
The content of above-described embodiment is only the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (4)
1. prepare a method for bismuth silicate powder, it is characterized in that comprising the following steps:
Take bismuth salt, water glass, reductive agent, the mol ratio of described bismuth salt, water glass, reductive agent is 1 ~ 12:1 ~ 2:10 ~ 30;
Water glass is dissolved in deionized water and obtains sodium silicate solution, and the concentration of described sodium silicate solution is between 0.5 ~ 2mol/L;
Reductive agent is dissolved in deionized water completely, obtains reductant solution;
Bismuth salt is dissolved in deionized water or salpeter solution completely, again sodium silicate solution and reductant solution are poured into, be heated to subsequently 80 ~ 100 DEG C, continue to stir after 3 ~ 10 minutes, direct solution immigration is heated in advance in the high temperature sintering furnace of 600 ~ 800 DEG C, along with the evaporation of moisture, obtain bismuth silicate powder.
2. a kind of method of preparing bismuth silicate powder as claimed in claim 1, is characterized in that: described bismuth salt is any one in Bismuth trinitrate, Bismuth carbonate.
3. a kind of method of preparing bismuth silicate powder as claimed in claim 1, is characterized in that: described reductive agent is any one in urea, citric acid, L-glutamic acid.
4. a kind of method of preparing bismuth silicate powder as claimed in claim 1, is characterized in that: the concentration of described salpeter solution is between 0.5 ~ 2mol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108479745A (en) * | 2018-03-05 | 2018-09-04 | 中山大学 | It is a kind of to modify bismuth silicate heterojunction photocatalyst and its preparation method and application certainly |
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|---|---|---|---|---|
| JP2004175643A (en) * | 2002-11-29 | 2004-06-24 | Yasushi Idemoto | Silicic acid-substituted ferroelectric oxide and its manufacturing method |
| JP2005276975A (en) * | 2004-03-24 | 2005-10-06 | Fuji Photo Film Co Ltd | Manufacturing method of photoconductive layer constituting radiation imaging panel |
| CN101157026A (en) * | 2007-11-08 | 2008-04-09 | 北京师范大学 | A preparation method of bismuth silicate powder photocatalyst |
| CN101780959A (en) * | 2010-02-09 | 2010-07-21 | 陕西科技大学 | Preparation method of Bi4Si3O12 nanocrystals |
| CN102351202A (en) * | 2011-07-06 | 2012-02-15 | 陕西科技大学 | Preparation method of bismuth silicate powder |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004175643A (en) * | 2002-11-29 | 2004-06-24 | Yasushi Idemoto | Silicic acid-substituted ferroelectric oxide and its manufacturing method |
| JP2005276975A (en) * | 2004-03-24 | 2005-10-06 | Fuji Photo Film Co Ltd | Manufacturing method of photoconductive layer constituting radiation imaging panel |
| CN101157026A (en) * | 2007-11-08 | 2008-04-09 | 北京师范大学 | A preparation method of bismuth silicate powder photocatalyst |
| CN101780959A (en) * | 2010-02-09 | 2010-07-21 | 陕西科技大学 | Preparation method of Bi4Si3O12 nanocrystals |
| CN102351202A (en) * | 2011-07-06 | 2012-02-15 | 陕西科技大学 | Preparation method of bismuth silicate powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108479745A (en) * | 2018-03-05 | 2018-09-04 | 中山大学 | It is a kind of to modify bismuth silicate heterojunction photocatalyst and its preparation method and application certainly |
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