CN108436101A - A kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres - Google Patents
A kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres Download PDFInfo
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Abstract
The present invention relates to a kind of methods of microwave radiation technology Fast back-projection algorithm Bi nanospheres, include the following steps (1)：It takes two water sodium bismuthate powder to be dissolved in ethylene glycol, two water bismuthic acid sodium solutions is made；(2)：It takes polyvinylpyrrolidone to be dissolved in ethylene glycol, polyvinylpyrrolidonesolution solution is made；(3)：It takes the polyvinylpyrrolidonesolution solution of step (2) to be added dropwise in two water bismuthic acid sodium solutions of step (1), stirs, form uniform mixed liquor；(4)：The uniform mixed liquor that microwave heating step (3) obtains, it is cooling, separation, washing, dry to get to purpose product.Compared with prior art, the present invention carries out reaction computer heating control using microwave and synthesizes bismuth nanosphere, simple for process, and synthesis is quick, and yield is higher etc..
Description
Technical field
The invention belongs to metal nano material technical fields, are related to a kind of side of microwave radiation technology Fast back-projection algorithm Bi nanospheres
Method.
Background technology
Metal nano material have unique physics, chemical property, photography, photonic propulsion, electronics, photoelectronics,
Sensor etc. has huge application potential.Bismuth belongs to the metal of indirect band gap, and the one kind generally acknowledged as the whole world is pacified very much
Complete, harmless " green metal ", in all metals (outside the removal of mercury), thermal conductivity is minimum, diamagnetism and Hall effect
Maximum is answered, effective electron mass is very small, and mean free path is longer.In addition, as a kind of semi-metallic, it had both had covalent
Key, and there is metallic bond, this unique structure makes it have unique performance.Bismuth metal adds in superconductor, lubricant oils
Agent, electrochemistry, thermoelectricity etc. is added to suffer from very important application.
Bismuth metal nano material has attracted the concern of numerous scholars due to unique performance.The bismuth metal nano reported
The synthesis of material has electrochemical process, template, solvent-thermal method, hydro-thermal method, liquid phase reduction etc..Although these methods can synthesize
Bismuth metal nano material have excellent performance, with specific structure, but there is also time-consuming, energy consumption, raw material are expensive and toxic
The shortcomings of.
Invention content
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of microwave radiation technology is quick
The method for synthesizing Bi nanospheres.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres, includes the following steps：
(1)：It takes two water sodium bismuthate powder to be dissolved in ethylene glycol, two water bismuthic acid sodium solutions is made；
(2)：It takes polyvinylpyrrolidone to be dissolved in ethylene glycol, polyvinylpyrrolidonesolution solution is made；
(3)：It takes the polyvinylpyrrolidonesolution solution of step (2) to be added dropwise in two water bismuthic acid sodium solutions of step (1), stirs
It mixes, forms uniform mixed liquor；
(4)：The uniform mixed liquor that microwave heating step (3) obtains, cooling, separation, washing, drying are produced to get to purpose
Object.
In a preferred embodiment, the addition ratio of two water sodium bismuthates and ethylene glycol is (0.3- in step (1)
0.6)g:(30-90)ml。
In a preferred embodiment, the addition ratio of polyvinylpyrrolidone and ethylene glycol is in step (2)
(1.2-3)g：(30-90)ml.
In a preferred embodiment, in step (3), polyvinylpyrrolidonesolution solution and two water bismuthic acid sodium solutions
Addition meets：The mass ratio of two water sodium bismuthates and polyvinylpyrrolidone is (0.3-0.6):(1.2-3).
In a preferred embodiment, in step (3), the time of stirring is 30-90min.In step (3), poly- second
The rate of addition control of alkene pyrrolidone solution is 1 drop/s.In this step, polyvinylpyrrolidonesolution solution is added dropwise to two water bismuthic acids
Speed and follow-up mixing time in sodium solution is suitable, if too fast or stirring dynamics and stirring is added in polyvinylpyrrolidone
Time is insufficient, then can cause two solution that cannot come into full contact with, and the target product pattern of formation is inhomogenous.
In a preferred embodiment, in step (4), the environment of microwave heating is provided by household microwave oven, heating
Program controls：5-10min is heated, rests 2-4min, it is 15-50min to be so recycled to accumulative heating time.It is furthermore preferred that
The model Galanz, P70F23P-G5 (SO) of household microwave oven, the microwave duration and degree of heating low, moderate heat and height fire in could be provided as.More
Preferably, in step (4), heating schedule control is：5-10min is heated, rests 2-4min, is so recycled to accumulative heating time
For 20min；The microwave heating duration and degree of heating is moderate heat.
In a preferred embodiment, in step (4), product separation, the process control washed are：It will be after cooling
Product is centrifuged with the rotating speed of 8000-10000r/min, is removed supernatant, required precipitation is obtained, then equipped with required precipitation
Ethyl alcohol and acetone are alternately added in centrifuge tube respectively, and with the rotating speed eccentric cleaning 4-7min of 8000-10000r/min.
In a preferred embodiment, in step (4), the process regulation of product drying is：With 50-70 DEG C
Temperature dries 12-18h.
In the present invention, the polyvinylpyrrolidone of addition is as dispersant, and effect is to be adsorbed on Bi nanometers of ball surfaces, resistance
The only contact between ball and ball, to prevent pelletizing combinate form at the particle of bigger, in step (1) and step (2), ethylene glycol is to make
Exist for solvent.Meanwhile after polyvinylpyrrolidonesolution solution is mixed with two water bismuthic acid sodium solutions, and in microwave heating treatment
In the process, chemical change can occur for each raw material component, and then generate Bi nanometers of ball materials, and specific reaction process is as follows：
HOCH2-CH2OH→CH3CHO+H2O；
5CH3CHO+2NaBiO3→2CH3COONa+3CH3COOH+2Bi+H2O。
, can be in microwave reaction if ethylene glycol is very few, solvent is evaporated, and reaction is caused to fail；If PVP it is excessive or
PVP solution injection rates are too fast, then excessively viscous PVP will be unable to evenly dispersed to solution, cause the pattern of product uneven；If
Microwave overlong time or the microwave duration and degree of heating are excessively high, then cause (1) Bi to be aoxidized, the pattern of (2) Bi it is uncontrollable.In order to realize the shape of Bi
Looks are uniform, and size is controllable, it is necessary to be subject to accurately to the amount of each reaction raw materials, PVP injection rates, the microwave duration and degree of heating and microwave time
Control.The amount of PVP cannot be excessive, and the injection rate of PVP will be controlled no more than 1 drop/s, otherwise probably because PVP disperses unevenness
It is even to cause last product morphology uneven.In addition, in order to control the size of Bi, microwave time and the duration and degree of heating are adjusted.Microwave fire
It waits and the time is unsuitable excessively high and long, otherwise will lead to the oxidation of Bi, the microwave duration and degree of heating is too low, then causes the pattern of Bi uneven
Even, the microwave duration and degree of heating is excessively high, although the fusing of bismuth will produce smaller Bi nanospheres, pattern is uneven.
Compared with prior art, the invention has the characteristics that：
(1) it is about thermoelectricity in 200nm that the bismuth metal that present invention microwave assisting method synthesizes, which has spherical structure, diameter,
The material preparation of material, lubricant material, the fields such as electrochemistry provides new method and new way, and is other inorganic compounds
Synthesis provides new approaches.
(2) mode of microwave heating of the invention may be implemented to heat simultaneously with surface inside reactant, meanwhile, microwave is anti-
It answers speed fast, preparation time is greatly saved, the energy is efficiently utilized.
(3) relative to other synthetic methods, microwave assisting method raw materials simple cheap, required technique is less, yield
It is higher, cost is greatly reduced, large-scale production is convenient for.
(4) nanocrystal can be designed, pattern, size are controllable.
Description of the drawings
Fig. 1 is the XRD diagram of the purpose product under different synthesis conditions produced by the present invention；
Fig. 2,3,4,6 are the SEM figures of the purpose product under different synthesis conditions produced by the present invention；
Fig. 5 is that the TEM of purpose product produced by the present invention schemes.
Specific implementation mode
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention
Premised on implemented, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to
Following embodiments.
Embodiment 1
The preparation of Bi nanometers of ball materials includes following steps：
Step 1: by bis- water sodium bismuthate (NaBiO of 0.3g3.2H2O it) is added into 30ml ethylene glycol, is stirred well to dissolving,
Obtain bismuthic acid sodium solution；
Step 2: 1.2g polyvinylpyrrolidones (PVP) are added into 30ml ethylene glycol, stirring to polyvinylpyrrolidine
Ketone dissolves, and solution becomes thick liquid, i.e. PVP solution；
Step 3: by PVP solution in the speed of 5 drops/s to bismuthic acid sodium solution, to stir in 90min, obtain mixed liquor；
Step 4: mixed liquor is transferred to household microwave oven (Galanz, P70F23P-G5 (SO)), low fire microwave is anti-in
10min is answered, then rests 3min, microwave reaction is continued with this operation order, finally microwave reaction 30min altogether.
Step 5: after being cooled to room temperature, product is centrifuged with the rotating speed of 8000r/min, removes supernatant, and it is required heavy to obtain
It forms sediment.Then ethyl alcohol and acetone are alternately added respectively in the centrifuge tube equipped with sediment, and clear with the centrifugation of the rotating speed of 8000r/min
Wash 6min.
15h is dried with 65 DEG C of temperature Step 6: finally the black product after cleaning is placed in vacuum drying chamber, is obtained
Target product Bi.
In the implementation case, final solvent evaporating completely, remaining black sticky end solid.This is because added ethylene glycol is very few
It is caused.
Embodiment 2
The preparation of Bi nanometers of ball materials includes following steps：
Step 1: by bis- water sodium bismuthate (NaBiO of 0.3g3.2H2O it) is added into 70ml ethylene glycol, is stirred well to dissolving；
Step 2: 1.2g polyvinylpyrrolidones (PVP) are added into 70ml ethylene glycol, stirring to polyvinylpyrrolidine
Ketone dissolves, and solution becomes thick liquid；
Step 3: PVP solution is injected into the speed of 5 drops/s in bismuthic acid sodium solution, stir in 90min；
Step 4: mixed liquor is transferred to household microwave oven (Galanz, P70F23P-G5 (SO)), low fire microwave is anti-in
10min is answered, then rests 3min, microwave reaction (last time microwave reaction 5min) is continued with this operation order, finally microwave altogether
React 35min.
Step 5: after being cooled to room temperature, product is centrifuged with the rotating speed of 8000r/min, removes supernatant, and it is required heavy to obtain
It forms sediment.Then ethyl alcohol and acetone are alternately added respectively in the centrifuge tube equipped with sediment, and clear with the centrifugation of the rotating speed of 8000r/min
Wash 6min.
15h is dried with 65 DEG C of temperature Step 6: finally the black product after cleaning is placed in vacuum drying chamber, is obtained
Target product Bi.
XRD characterization is carried out to the product in the present embodiment, finally shows that result is pure Bi (Fig. 1)；Shape is carried out to it again
Looks characterize, and display result is irregular pattern.This is because the injection of PVP solution is too fast, great viscosity makes it can not be with bismuth
Acid sodium solution is sufficiently mixed, and leads to the uneven of pattern.
Embodiment 3
The preparation of Bi nanometers of ball materials includes following steps：
Step 1: by bis- water sodium bismuthate (NaBiO of 0.4g3.2H2O it) is added into 70ml ethylene glycol, is stirred well to dissolving；
Step 2: 1.2g polyvinylpyrrolidones (PVP) are added into 70ml ethylene glycol, stirring to polyvinylpyrrolidine
Ketone dissolves, and solution becomes thick liquid；
Step 3: PVP solution is dropped to the rate of 1 drop/s in bismuthic acid sodium solution, stir in 60min；
Step 4: mixed liquor is transferred to household microwave oven (Galanz, P70F23P-G5 (SO)), low fire microwave is anti-in
10min is answered, then rests 3min, microwave reaction (last time microwave reaction 5min) is continued with this operation order, finally microwave altogether
React 35min.
Step 5: after being cooled to room temperature, product is centrifuged with the rotating speed of 8000r/min, removes supernatant, and it is required heavy to obtain
It forms sediment.Then ethyl alcohol and acetone are alternately added respectively in the centrifuge tube equipped with sediment, and clear with the centrifugation of the rotating speed of 8000r/min
Wash 6min.
17h is dried with 60 DEG C of temperature Step 6: finally the black product after cleaning is placed in vacuum drying chamber, is obtained
Target product Bi.
To the product X RD tests in the present embodiment, it is found that it is pure Bi；Morphology characterization is carried out to it again, Fig. 2 is it
SEM schemes, and it is not especially uniformly to find its pattern also.This may be since the microwave duration and degree of heating and microwave time are improper caused.
Embodiment 4
The preparation of Bi nanometers of ball materials includes following steps：
Step 1: by bis- water sodium bismuthate (NaBiO of 0.4g3.2H2O it) is added into 70ml ethylene glycol, is stirred well to dissolving；
Step 2: 1.6g polyvinylpyrrolidones (PVP) are added into 70ml ethylene glycol, stirring to polyvinylpyrrolidine
Ketone dissolves, and solution becomes thick liquid；
Step 3: PVP solution is dropped to the rate of 1 drop/s in bismuthic acid sodium solution, stir in 60min；
Step 4: mixed liquor is transferred to household microwave oven (Galanz, P70F23P-G5 (SO)), low fire microwave is anti-in
10min is answered, then rests 3min, microwave reaction is continued with this operation order, finally microwave reaction 50min altogether.
Step 5: after being cooled to room temperature, product is centrifuged with the rotating speed of 8000r/min, removes supernatant, and it is required heavy to obtain
It forms sediment.Then ethyl alcohol and acetone are alternately added respectively in the centrifuge tube equipped with sediment, and clear with the centrifugation of the rotating speed of 8000r/min
Wash 5min.
18h is dried with 60 DEG C of temperature Step 6: finally the black product after cleaning is placed in vacuum drying chamber, is obtained
Target product Bi.
To the product X RD tests in the present embodiment, it is found that it is pure Bi (Fig. 1)；Morphology characterization, Fig. 3 are carried out to it again
Scheme for its SEM, it is not especially uniform to find its pattern also, and the 35min synthesis of particle ratio is small.When this may be due to microwave
Between long the Bi of low melting point is caused to melt.
Embodiment 5
The preparation of Bi nanometers of ball materials includes following steps：
Step 1: by bis- water sodium bismuthate (NaBiO of 0.6g3.2H2O it) is added into 90ml ethylene glycol, is stirred well to dissolving；
Step 2: 1.8g polyvinylpyrrolidones (PVP) are added into 90ml ethylene glycol, stirring to polyvinylpyrrolidine
Ketone dissolves, and solution becomes thick liquid；
Step 3: PVP solution is dropped to the rate of 1 drop/s in bismuthic acid sodium solution, stir in 90min；
Step 4: mixed liquor is transferred to household microwave oven (Galanz, P70F23P-G5 (SO)), with moderate heat microwave reaction
10min, then rest 4min, continues microwave reaction with this operation order, finally microwave reaction 20min altogether.
Step 5: after being cooled to room temperature, product is centrifuged with the rotating speed of 8000r/min, removes supernatant, and it is required heavy to obtain
It forms sediment.Then ethyl alcohol and acetone are alternately added respectively in the centrifuge tube equipped with sediment, and clear with the centrifugation of the rotating speed of 8000r/min
Wash 5min.
18h is dried with 60 DEG C of temperature Step 6: finally the black product after cleaning is placed in vacuum drying chamber, is obtained
Target product Bi.
To the product X RD tests in the present embodiment, it is found that it is pure Bi (Fig. 1)；Morphology characterization, Fig. 4 are carried out to it again
Scheme for its SEM, Fig. 5 schemes for its TEM, it is found that its pattern is spherical shape, diameter is in 200nm or so.
Embodiment 6
The preparation of Bi nanometers of ball materials includes following steps：
Step 1: by bis- water sodium bismuthate (NaBiO of 0.45g3.2H2O it) is added into 80ml ethylene glycol, is stirred well to molten
Solution；
Step 2: 1.8g polyvinylpyrrolidones (PVP) are added into 80ml ethylene glycol, stirring to polyvinylpyrrolidine
Ketone dissolves, and solution becomes thick liquid；
Step 3: PVP solution is dropped to the rate of 1 drop/s in bismuthic acid sodium solution, stir in 90min；
Step 4: mixed liquor is transferred to household microwave oven (Galanz, P70F23P-G5 (SO)), with moderate heat microwave reaction
10min, then rest 4min, continues microwave reaction with this operation order, finally microwave reaction 30min altogether.
Step 5: after being cooled to room temperature, product is centrifuged with the rotating speed of 8000r/min, removes supernatant, and it is required heavy to obtain
It forms sediment.Then ethyl alcohol and acetone are alternately added respectively in the centrifuge tube equipped with sediment, and clear with the centrifugation of the rotating speed of 8000r/min
Wash 5min.
12h is dried with 70 DEG C of temperature Step 6: finally the black product after cleaning is placed in vacuum drying chamber, is obtained
Target product Bi.
To the product X RD tests in the present embodiment, it is found that it is pure Bi (Fig. 1)；Morphology characterization, Fig. 6 are carried out to it again
For its SEM scheme, find pattern it is irregular, and compared under moderate heat the Bi particles of microwave 20min want small.This is because improper
The microwave time caused by.The microwave time is longer to cause temperature excessively high, to destroy the pattern of Bi.
Embodiment 7
The preparation of Bi nanometers of ball materials includes following steps：
Step 1: by bis- water sodium bismuthate (NaBiO of 0.4g3.2H2O it) is added into 80ml ethylene glycol, is stirred well to dissolving；
Step 2: 2g polyvinylpyrrolidones (PVP) are added into 80ml ethylene glycol, stirring to polyvinylpyrrolidone
Dissolving, solution become thick liquid；
Step 3: PVP solution is dropped to the rate of 1 drop/s in bismuthic acid sodium solution, stir in 60min；
Step 4: mixed liquor is transferred to household microwave oven (Galanz, P70F23P-G5 (SO)), with high fiery microwave reaction
5min, then rest 4min, continues microwave reaction with this operation order, finally microwave reaction 15min altogether.
Step 5: after being cooled to room temperature, product is centrifuged with the rotating speed of 8000r/min, removes supernatant, and it is required heavy to obtain
It forms sediment.Then ethyl alcohol and acetone are alternately added respectively in the centrifuge tube equipped with sediment, and clear with the centrifugation of the rotating speed of 8000r/min
Wash 5min.
12h is dried with 70 DEG C of temperature Step 6: finally the black product after cleaning is placed in vacuum drying chamber, is obtained
Faint yellow product.
XRD tests are carried out to the product in the present embodiment, it is found that it is Bi2O3.Cause Bi by oxygen this is because temperature is excessively high
Change.
Embodiment 8
Compared with Example 5, the overwhelming majority is all identical, in addition in the present embodiment step 2, polyvinylpyrrolidone adds
It is 3g to enter amount.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiment without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be the present invention's
Within protection domain.
Claims (10)
1. a kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres, which is characterized in that include the following steps：
(1)：It takes two water sodium bismuthate powder to be dissolved in ethylene glycol, two water bismuthic acid sodium solutions is made；
(2)：It takes polyvinylpyrrolidone to be dissolved in ethylene glycol, polyvinylpyrrolidonesolution solution is made；
(3)：It takes the polyvinylpyrrolidonesolution solution of step (2) to be added dropwise in two water bismuthic acid sodium solutions of step (1), stirs, shape
At uniform mixed liquor；
(4)：The uniform mixed liquor that microwave heating step (3) obtains, it is cooling, separation, washing, dry to get to purpose product.
2. a kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres according to claim 1, which is characterized in that step
(1) the addition ratio of two water sodium bismuthates and ethylene glycol is (0.3-0.6) g in:(30-90)ml.
3. a kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres according to claim 1, which is characterized in that step
(2) the addition ratio of polyvinylpyrrolidone and ethylene glycol is (1.2-3) g in：(30-90)ml.
4. a kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres according to claim 1, which is characterized in that step
(3) in, polyvinylpyrrolidonesolution solution and the addition of two water bismuthic acid sodium solutions meet：Two water sodium bismuthates and polyvinylpyrrolidine
The mass ratio of ketone is (0.3-0.6):(1.2-3).
5. a kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres according to claim 1, which is characterized in that step
(3) in, the time of stirring is 30-90min.
6. a kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres according to claim 1, which is characterized in that step
(3) in, the rate of addition of polyvinylpyrrolidonesolution solution is 1 drop/s.
7. a kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres according to claim 1, which is characterized in that step
(4) in, the environment of microwave heating is provided by household microwave oven, and heating schedule control is：5-10min is heated, rests 2-4min, such as
This is recycled to accumulative heating time as 15-50min.
8. a kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres according to claim 7, which is characterized in that step
(4) in, heating schedule control is：5-10min is heated, rests 2-4min, it is 20min to be so recycled to accumulative heating time；
The microwave heating duration and degree of heating is moderate heat.
9. a kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres according to claim 1, which is characterized in that step
(4) in, product separation, the process control washed are：Product after cooling is centrifuged with the rotating speed of 8000-10000r/min, is gone
Except supernatant, required precipitation is obtained, is then alternately added ethyl alcohol and acetone respectively in the centrifuge tube equipped with required precipitation, and with
The rotating speed eccentric cleaning 4-7min of 8000-10000r/min.
10. a kind of method of microwave radiation technology Fast back-projection algorithm Bi nanospheres according to claim 1, which is characterized in that step
(4) in, the process regulation of product drying is：12-18h is dried with 50-70 DEG C of temperature.
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| CN110653380A (en) * | 2019-10-31 | 2020-01-07 | 合肥工业大学 | Method for rapidly preparing gold nanoparticles in alcohol phase at normal temperature |
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