CN105908214A - Preparation method for pure metal bismuth nanoparticles - Google Patents
Preparation method for pure metal bismuth nanoparticles Download PDFInfo
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- CN105908214A CN105908214A CN201610409789.5A CN201610409789A CN105908214A CN 105908214 A CN105908214 A CN 105908214A CN 201610409789 A CN201610409789 A CN 201610409789A CN 105908214 A CN105908214 A CN 105908214A
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- bismuth
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/22—Electrolytic production, recovery or refining of metals by electrolysis of solutions of metals not provided for in groups C25C1/02 - C25C1/20
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention provides a preparation method for pure metal bismuth nanoparticles and belongs to the technical filed of metal nano material preparation. The preparation method comprises the following steps that bismuth elements in chloride salt containing bismuth are uniformly deposited in hole channels of a porous alumina mold plate, so that pure metal bismuth nanowire arrays are obtained; the porous alumina mold plate fully deposited with pure metal bismuth nanowires is connected with a wire with conductive silver paste, so that an electrode is made; then the electrode is connected into an experimental circuit in series, the direct current voltage is set to be 40 V, the experiment time is set to be 60 min, and the experiment process is repeated for two to three times; and a measured sample cross section is selected to be observed through a scanning electron microscope, and thus it can be found that the particle refinement phenomenon appears on the pure metal bismuth nanowires along with increasing of the times of the repeated experiments. According to the preparation method for the pure metal bismuth nanoparticles, the preparation process is simple, and the raw materials are easy to obtain; the voltage and the time of experimental reaction are controllable; and in addition, the prepared materials are widely applied to thermoelectricity, lubricating oil additives and other aspects.
Description
Technical field
The present invention relates to metal nano material preparation field, be specifically related to a kind of elemental metals bismuth nano-particle system
Preparation Method, belongs to metal nano material preparing technical field.
Background technology
Metal nano material not only has the characteristic of metal itself and nano material, also has quite simultaneously
Excellent process based prediction model, therefore, metal nano material has been increasingly becoming in the research of material supply section educational circles
The heart.And the ratio of the surface atom of the metal nanoparticle in metal nano material and total atom number is along with particle diameter
Reduce and increase, demonstrate strong bulk effect, quantum size effect, skin effect and macroscopic quantum tunnel
Channel effect.Metal nanoparticle has been widely used for catalysis, photocatalysis, information stores, surface enhanced draws
The field such as graceful, solaode and optoelectronics.Therefore, the preparation to metal nanoparticle is that everybody pays close attention to
Emphasis.
Bismuth is a kind of semi-metallic with indirect band gap energy, has the electrical properties of uniqueness.Because bismuth
Fermi surface high anisotropy, and conduction band and Valence-band is a little overlapping so that each in valence band and conduction band
From producing hole and two kinds of carriers of electronics, the two carrier concentration is little, and effective mass is the least, flat
All free paths are the longest, and mobility is high.Routine prepares the method for metal nanoparticle has hydro-thermal method, aqueous solution also
Former method and precipitation transformation method etc..Hydro-thermal method can directly obtain dispersion and the powder body of well-crystallized, it is not necessary to does
High temperature sintering processes, it is to avoid may the powder body hard aggregation of stroke.The particle dispersion that aqueous solution reducing process obtains
Property is good, and grain shape is the most spherical in shape, and process can also control.Precipitation transformation method technological process is short, operation
Simplicity, but the compound of preparation is only limitted to a few metals oxide and hydroxide.This patent will describe
A kind of method of preparing elemental metals nano-particle of simple and fast.
Summary of the invention
It is an object of the invention to provide a kind of simple method and prepare elemental metals bismuth nano-particle.
To achieve these goals, the present invention is by the following technical solutions: first with porous alumina formwork be
Carrier, the full elemental metals bismuth nano-wire array of deposition, it is connected by conductive silver paste with wire and accesses direct current
In circuit, increase sample experiment number in fusing recrystallization process and i.e. can get elemental metals bismuth nanometer
The phenomenon of grain.
The preparation method of a kind of elemental metals bismuth nano-particle, it is characterised in that step is as follows:
(1) prepared by elemental metals bismuth nano-wire array:
Porous alumina formwork is placed in the aqueous solution of the chlorate containing bismuth as cathode material, graphite electricity
Pole, as anode material, uses the method for unidirectional current chemical deposition to prepare, constant temperature 0 DEG C reaction 8h, unidirectional current
Pressure size is 1.3-1.5V, obtains depositing the porous alumina formwork of elemental metals bismuth nano-wire array；
(2) repeatedly melt under the conditions of extra electric field recrystallization formed elemental metals bismuth nano-particle:
The porous alumina formwork that deposition has elemental metals bismuth nano-wire array uses conductive silver paste and wire phase
Even, and in insert experiment circuit, in the environment of room temperature, under conditions of DC voltage is 40V, continue
Fusing 60min, after recrystallization completes, identical under conditions of repeat experimental implementation 2～3 times, will be containing singly
The porous alumina formwork of matter bismuth metal nanometer line array selects its cross section to be scanned ultramicroscope sight
Survey, the elemental metals bismuth nano-particle obtained can be found.
Further, the chlorate aqueous solution of described bismuth be by two trichloride hydrate bismuths, tartaric acid, citric acid,
Trisodium citrate, glycerol and sodium chloride are dissolved in distilled water, and stirring forms transparent solution and makes, Qi Zhongfen
Do not take two trichloride hydrate bismuth molar concentrations to be 0.04M, take tartaric acid molar concentration and be 0.1M, take citric acid
Molar concentration is 0.2M, take trisodium citrate molar concentration is 0.1M, take glycerol molar concentration is 0.88M
It is 1.2M with sodium chloride molar concentration.
Further, the chlorate aqueous solution hydrochloric acid of described bismuth or the pH value of ammonia regulation solution, make solution
PH value be 1.
Along with the increase of repeated melting recrystallization number of operations, the elemental metals bismuth nano-particle obtained occurs
Phenomenon is more and more obvious.
The invention has the beneficial effects as follows: the raw material of the inventive method is easily obtained, preparation technology is simple, voltage
Size and reaction temperature, time are controlled, and the nano-particle of preparation is prone to find observation.
Accompanying drawing explanation
Fig. 1 is that the X of the elemental metals bismuth nano-wire array prepared in porous alumina formwork hole penetrates
Line diffraction (XRD) figure.
Fig. 2 is under the conditions of DC voltage 40V, and the time dependent song of resistance of three times measured respectively by sample
Line chart.
Fig. 3 is that for the first time the scanning electron microscope (SEM) of elemental metals bismuth nano-wire is shone after fusing recrystallization
Sheet.
Fig. 4 is that after second time melts recrystallization, the scanning electron microscope (SEM) of elemental metals bismuth nano-wire is shone
Sheet.
Fig. 5 is that after third time melts recrystallization, the scanning electron microscope (SEM) of elemental metals bismuth nano-wire is shone
Sheet.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail.
First 3.525g bis-chloride hydrate bismuth, 3.75g tartaric acid, 10.25g Fructus Citri Limoniae are taken with electronic balance weighing
Acid trisodium, 7.35g citric acid, 20.25g glycerol and 18g sodium chloride are stand-by, measure 250ml with graduated cylinder
Ionized water is poured in the beaker of magneton, and is placed on magnetic stirring apparatus stirring, then according to tartaric acid,
The sequencing of citric acid, trisodium citrate, glycerol and sodium chloride is poured into successively in beaker and is stirred to the most molten
Solve, regulate the pH value of solution with hydrochloric acid or ammonia, make the pH value of solution be adjusted to 1.
Using graphite electrode as anode material, porous alumina formwork, as cathode material, preparation-obtained contains
There is the chlorate solution of bismuth as electrolyte, under the constant temperature of 0 DEG C, under the DC voltage of 1.3-1.5V,
Long-time deposition, the time is about 8h, obtains filling out in porous alumina formwork and is filled with elemental metals bismuth nano-wire
Array.Deposition has the porous anodic alumina template of elemental metals bismuth nano-wire array corresponding to standard card Bi
X-ray diffraction (XRD) figure of (JCPDS Card No.44-1246) is as shown in Figure 1.
By the porous alumina formwork both sides dropping conductive silver serosity of full for deposition elemental metals bismuth nano-wire array
Drip, and be connected with wire, after wire is fixed by conductive silver paste completely with porous anodic alumina template,
It is connected in experimental circuit.
Under conditions of DC voltage 40V, carry out test 60min, certain interval of time until sample cool down after,
Sample carrying out second time and third time repeats experiment, experiment condition is identical with experiment condition last time.Fig. 2
Under the conditions of DC voltage 40V, the resistance versus time curve figure of three times measured respectively by sample, permissible
See that resistance increases over time in the trend risen, the most all reached a relatively steady state,
Cycle-index is the most more easily reaches relatively steady state.
Cross section is selected to be scanned ultramicroscope in the porous alumina formwork sample after experiment terminates every time
Observation, Fig. 3 is the scanning electron microscope after the elemental metals bismuth nano-wire fusing recrystallization for the first time of preparation
(SEM) photo, it appeared that the bismuth with elementary metal nanometer line being deposited in porous alumina formwork duct occurs in that
A small amount of phenomenon of rupture.Fig. 4 is the scanning after the elemental metals bismuth nano-wire second time fusing recrystallization of preparation
Ultramicroscope (SEM) photo, it appeared that the bismuth with elementary metal being deposited in porous alumina formwork duct is received
Rice noodle is fractured into short and small nanometer stub.Fig. 5 is that the elemental metals bismuth nano-wire third time fusing of preparation is tied again
Scanning electron microscope (SEM) photo after crystalline substance, it appeared that the list being deposited in porous alumina formwork duct
Matter bismuth metal nanometer line final fracture is tiny bismuth with elementary nano-particle.From accompanying drawing 3 to accompanying drawing 5,
Along with the increase of repeated melting recrystallization number of times, the phenomenon that the elemental metals bismuth nano-particle obtained occurs more is come
The most obvious.
Claims (4)
1. the preparation method of an elemental metals bismuth nano-particle, it is characterised in that step is as follows:
(1) prepared by elemental metals bismuth nano-wire array:
Porous alumina formwork is placed into containing in the aqueous solution of the chlorate of bismuth as cathode material, graphite
Electrode, as anode material, uses the method for unidirectional current chemical deposition to prepare, constant temperature 0 DEG C reaction 8h, direct current
Voltage swing is 1.3-1.5V, obtains depositing the porous alumina formwork of elemental metals bismuth nano-wire array；
(2) repeatedly melt under current field condition recrystallization formed elemental metals bismuth nano-particle:
The porous alumina formwork that deposition has elemental metals bismuth nano-wire array uses conductive silver paste and wire phase
Even, and in insert experiment circuit, in the environment of room temperature, under conditions of DC voltage is 40V, continue
Heating 60min, after recrystallization to be melted completes, identical under conditions of repeat experimental implementation 2～3 times, will contain
The porous alumina formwork having bismuth with elementary metal nanometer line array selects its cross section to be scanned ultramicroscope
Observation, can find the elemental metals bismuth nano-particle obtained.
The preparation method of elemental metals bismuth nano-particle the most according to claim 1, it is characterised in that:
The chlorate aqueous solution of described bismuth be by two trichloride hydrate bismuths, tartaric acid, citric acid, trisodium citrate,
Glycerol and sodium chloride are dissolved in distilled water, and stirring forms transparent solution and makes, and takes two hydrations three the most respectively
Bismuth chloride molar concentration is 0.04M, take tartaric acid molar concentration is 0.1M, take citric acid molar concentration is
0.2M, take sodium citrate molar concentration be 0.1M, to take glycerol molar concentration be 0.88M and sodium chloride mole
Concentration is 1.2M.
The preparation method of elemental metals bismuth nano-particle the most according to claim 2, it is characterised in that:
The chlorate aqueous solution hydrochloric acid of described bismuth or the pH value of ammonia regulation solution, the pH value making solution is 1.
The preparation method of elemental metals bismuth nano-particle the most according to claim 1, it is characterised in that:
Along with the increase of repetition experimental implementation number of times in step (2), the elemental metals bismuth nano-particle obtained occurs
Phenomenon is more and more obvious.
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| CN201610409789.5A CN105908214A (en) | 2016-06-08 | 2016-06-08 | Preparation method for pure metal bismuth nanoparticles |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106711254A (en) * | 2016-12-26 | 2017-05-24 | 电子科技大学 | Method of preparing diameter-adjustable bismuth nanowire array |
| CN106981650A (en) * | 2017-02-10 | 2017-07-25 | 中山大学 | A kind of preparation method of nanoscale bismuth with elementary |
| CN107282933A (en) * | 2017-05-17 | 2017-10-24 | 华东师范大学 | A kind of preparation method of dry method bismuth nano particle |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101569934A (en) * | 2009-05-27 | 2009-11-04 | 河南大学 | Method for preparing metal bismuth nanoparticle |
| CN104668578A (en) * | 2015-02-05 | 2015-06-03 | 北京理工大学 | Preparation method for bismuth nanometer particles |
-
2016
- 2016-06-08 CN CN201610409789.5A patent/CN105908214A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101569934A (en) * | 2009-05-27 | 2009-11-04 | 河南大学 | Method for preparing metal bismuth nanoparticle |
| CN104668578A (en) * | 2015-02-05 | 2015-06-03 | 北京理工大学 | Preparation method for bismuth nanometer particles |
Non-Patent Citations (1)
| Title |
|---|
| 何朝成: "铋、铅及其合金纳米线在焦耳自加热过程中的融化行为", 《中国优秀硕士论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106711254A (en) * | 2016-12-26 | 2017-05-24 | 电子科技大学 | Method of preparing diameter-adjustable bismuth nanowire array |
| CN106981650A (en) * | 2017-02-10 | 2017-07-25 | 中山大学 | A kind of preparation method of nanoscale bismuth with elementary |
| CN107282933A (en) * | 2017-05-17 | 2017-10-24 | 华东师范大学 | A kind of preparation method of dry method bismuth nano particle |
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