CN104192854B - A kind of method preparing bismuth silicate powder - Google Patents
A kind of method preparing bismuth silicate powder Download PDFInfo
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- CN104192854B CN104192854B CN201410317866.5A CN201410317866A CN104192854B CN 104192854 B CN104192854 B CN 104192854B CN 201410317866 A CN201410317866 A CN 201410317866A CN 104192854 B CN104192854 B CN 104192854B
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- bismuth
- sodium silicate
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Abstract
A kind of method preparing bismuth silicate powder of the present invention, comprises the following steps: to take bismuth salt, water glass, reductive agent, and the mol ratio of described bismuth salt, water glass, reductive agent is 1 ~ 12:1 ~ 2:10 ~ 30; Dissolved by water glass and obtain sodium silicate solution in deionized water, the concentration of described sodium silicate solution is between 0.5 ~ 2mol/L; Reductive agent is dissolved completely in deionized water, obtains reductant solution; Bismuth salt is dissolved completely in deionized water or salpeter solution, again sodium silicate solution and reductant solution are poured into, 80 ~ 100 DEG C are heated to subsequently with magnetic stirring apparatus, after Keep agitation, being moved into by solution is heated in the high temperature sintering furnace of 600 ~ 800 DEG C in advance, along with the evaporation of moisture, vigorous combustion, obtains fluffy spumescence product.The present invention adopts the water glass of cost cheaper to be raw material, is conducive to practical application; Obtained powder good dispersion, particle is tiny; Equipment, technique are simple.
Description
Technical field
The invention belongs to inorganic non-metallic ultrafine powder field, particularly relate to a kind of bismuth silicate powder, specifically a kind of method preparing bismuth silicate powder.
Background technology
Different with the content of silicon according to bismuth in compound, bismuth silicate is mainly divided into two classes, and one is Bi
4si
3o
12, one is Bi
12siO
20.The former is a kind of important scintillation crystal, it and the bismuth germanium oxide (Bi to be 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 of alternative 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 is the non-ferroelectric cubic oxide thing crystal simultaneously with the effect such as electricity, photoconduction, Preset grating, piezoelectricity and opticity and Faraday optically-active, has a wide range of applications in light amplification, phase conjugate compensation, Hologram Storage, image processing and surface acoustic wave device etc.
Obtain high-quality crystalline material or transparent ceramic material, raw material primarily solves 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 grain of acquisition is comparatively thick, needs follow-up pulverizing process could be levigate by product.Sol-gel method is a kind of emerging wet chemical synthesis, although obtained powder 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 preparing bismuth silicate powder, it is not only expensive that the described this method 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 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 dissolving is obtained sodium silicate solution in deionized water, the concentration of described sodium silicate solution is between 0.5 ~ 2mol/L;
3) reductive agent is dissolved completely in deionized water, obtains reductant solution;
4) bismuth salt is dissolved completely in deionized water or salpeter solution, again sodium silicate solution and reductant solution are poured into, be heated to 80 ~ 100 DEG C subsequently, Keep agitation is after 3 ~ 10 minutes, solution is directly moved in the high temperature sintering furnace being heated to 600 ~ 800 DEG C in advance, 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 for raw material with sodium silicate solution and adopts combustion synthesis technology to prepare, and thus there is not the problems such as sol-gel method expensive starting materials, technique are loaded down with trivial details, thus has with low cost, the simple technique effect of technique.
The present invention does not need external heat source long duration of action, therefore there is not the problems such as sintering temperature is higher, long reaction time, the technique effect that thus to have that thermal treatment temp is low, quick, product is reunited few.
Present invention employs combustion synthesis method, thus there is not the problems such as solid state sintering needs external heat source and sol-gel method technique is loaded down with trivial details, thus there is efficiency high, be conducive to reducing manufacturing cost, be easy to the technique effect of industrialization.
The present invention compares with prior art, and its technical progress is significant.The present invention adopts the water glass of cost cheaper to be raw material, is conducive to practical application; Obtained powder good dispersion, particle is tiny; Equipment, technique are simple.
Accompanying drawing explanation
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, dissolved by water glass and obtain sodium silicate solution in deionized water, the concentration of silicon sodium solution is at 0.5mol/L, is dissolved completely in deionized water by urea.Bismuth trinitrate is dissolved completely in deionized water, again sodium silicate solution and urea soln are poured into, be heated to 80 DEG C with magnetic stirring apparatus subsequently, solution, after 3 minutes, directly moves in the high temperature sintering furnace being heated to 750 DEG C in advance by Keep agitation, along with the evaporation of moisture, vigorous combustion, obtains fluffy spumescence product, and itself XRD and SEM schemes respectively as depicted in figs. 1 and 2, from XRD figure, product is bismuth silicate (Bi substantially
4si
3o
12) phase, as can be seen from SEM figure, the median size of silicic acid bismuth meal is 0.25 μm.
Embodiment 2
In Bismuth trinitrate: water glass: urea=4:3:26 ratio batching, dissolved by water glass and obtain sodium silicate solution in deionized water, the concentration of sodium silicate solution is at 1.5mol/L, is dissolved completely in deionized water by urea.Bismuth trinitrate is dissolved completely in deionized water, again sodium silicate solution and urea soln are poured into, 100 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 5 minutes, solution is directly moved in the high temperature sintering furnace being heated to 600 DEG C in advance, all the other implementation conditions, all with embodiment 1, obtain the bismuth silicate (Bi that median size is about 0.18 μm
4si
3o
12) powder.
Embodiment 3
In bismuth hydroxide: water glass: urea=4:3:10 ratio batching, dissolved by water glass and obtain sodium silicate solution in deionized water, the concentration of sodium silicate solution is at 0.5mol/L, is dissolved completely in deionized water by urea.Bismuth hydroxide is dissolved completely in nitric acid, again sodium silicate solution and urea soln are poured into, 100 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 10 minutes, solution is directly moved in the high temperature sintering furnace being heated to 800 DEG C in advance, all the other implementation conditions, all with embodiment 1, obtain the bismuth silicate (Bi that median size is about 0.32 μm
4si
3o
12) powder.
Embodiment 4
In Bismuth carbonate: water glass: urea=4:3:28 ratio batching, dissolved by water glass and obtain sodium silicate solution in deionized water, the concentration of sodium silicate solution is at 0.5mol/L, is dissolved completely in deionized water by urea.Bismuth carbonate is dissolved completely in nitric acid, again sodium silicate solution and urea soln are poured into, 100 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 3 minutes, solution is directly moved in the high temperature sintering furnace being heated to 800 DEG C in advance, all the other implementation conditions, all with embodiment 1, obtain the bismuth silicate (Bi that median size is about 0.24 μm
4si
3o
12) powder.
Embodiment 5
In Bismuth trinitrate: water glass: urea=12:1:30 ratio batching, dissolved by water glass and obtain sodium silicate solution in deionized water, the concentration of sodium silicate solution is at 1.5mol/L, is dissolved completely in deionized water by urea.Bismuth carbonate is dissolved completely in nitric acid, again sodium silicate solution and urea soln are poured into, 100 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 3 minutes, solution is directly moved in the high temperature sintering furnace being heated to 800 DEG C in advance, all the other implementation conditions, all with embodiment 1, obtain the bismuth silicate (Bi that median size is about 0.28 μm
12siO
20) powder.
Embodiment 6
In Bismuth trinitrate: water glass: citric acid=4:3:4 ratio batching, dissolved by water glass and obtain sodium silicate solution in deionized water, the concentration of sodium silicate solution is at 0.5mol/L, is dissolved completely in deionized water by citric acid.Bismuth trinitrate is dissolved completely in deionized water, again sodium silicate solution and citric acid solution are poured into, 100 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 3 minutes, solution is directly moved in the high temperature sintering furnace being heated to 800 DEG C in advance, all the other implementation conditions, all with embodiment 1, obtain the bismuth silicate (Bi that median size is about 0.24 μm
4si
3o
20) powder.
Embodiment 7
In Bismuth trinitrate: water glass: L-glutamic acid=4:3:26 ratio batching, dissolved by water glass and obtain sodium silicate solution in deionized water, the concentration of sodium silicate solution is at 0.5mol/L, is dissolved completely in deionized water by L-glutamic acid.Bismuth trinitrate is dissolved completely in deionized water, again sodium silicate solution and glutamic acid solution are poured into, 80 DEG C are heated to subsequently with magnetic stirring apparatus, Keep agitation is after 3 minutes, solution is directly moved in the high temperature sintering furnace being heated to 700 DEG C in advance, all the other implementation conditions, all with embodiment 1, obtain the bismuth silicate (Bi that median size is about 0.26 μm
4si
3o
12) powder.
The content of above-described embodiment be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.
Claims (2)
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; Described bismuth salt is any one in Bismuth trinitrate, Bismuth carbonate, and described reductive agent is urea;
Dissolved by water glass and obtain sodium silicate solution in deionized water, the concentration of described sodium silicate solution is between 0.5 ~ 2mol/L;
Reductive agent is dissolved completely in deionized water, obtains reductant solution;
Bismuth salt is dissolved completely in deionized water or salpeter solution, again sodium silicate solution and reductant solution are poured into, be heated to 80 ~ 100 DEG C subsequently, Keep agitation is after 3 ~ 10 minutes, solution is directly moved in the high temperature sintering furnace being heated to 600 ~ 800 DEG C in advance, along with the evaporation of moisture, obtain bismuth silicate powder, the molecular formula of described bismuth silicate powder is Bi
4si
3o
12.
2. a kind of method preparing bismuth silicate powder as claimed in claim 1, is characterized in that: described salpeter solution dense
Degree is between 0.5 ~ 2mol/L.
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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 |
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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 |
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