CN101824625A - Method for controllably synthesizing bismuth-based nano-material by directly electrolyzing metal bismuth - Google Patents
Method for controllably synthesizing bismuth-based nano-material by directly electrolyzing metal bismuth Download PDFInfo
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- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 41
- 229910052751 metal Inorganic materials 0.000 title abstract description 15
- 239000002184 metal Substances 0.000 title abstract description 15
- 230000002194 synthesizing effect Effects 0.000 title abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 132
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 46
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 44
- 239000011780 sodium chloride Substances 0.000 claims abstract description 22
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012153 distilled water Substances 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000000243 solution Substances 0.000 claims description 33
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 21
- 239000008151 electrolyte solution Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 7
- 239000013077 target material Substances 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 abstract description 20
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000003792 electrolyte Substances 0.000 abstract 3
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 abstract 1
- 238000010923 batch production Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 60
- 238000005260 corrosion Methods 0.000 description 20
- 230000007797 corrosion Effects 0.000 description 20
- 229910000474 mercury oxide Inorganic materials 0.000 description 16
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical class [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 16
- 239000011858 nanopowder Substances 0.000 description 13
- 238000005406 washing Methods 0.000 description 7
- 239000002244 precipitate Substances 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- -1 bismuth oxide compound Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 229910000416 bismuth oxide Inorganic materials 0.000 description 3
- 238000009388 chemical precipitation Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229940073609 bismuth oxychloride Drugs 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000593 microemulsion method Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention discloses a method for controllably synthesizing a bismuth-based nano-material by directly electrolyzing metal bismuth. In the electrolysis process of the method, metal bismuth serves as a sacrificial anode, mixed aqueous solution of sodium chloride, disodium ethylene diamine tetraacetic acid and sodium hydroxide serves as electrolyte, direct current is electrified for electrolyzing, and the proportion of electrolyte components is adjusted so as to prepare the bismuth-base nano-material. The method has the advantages of cheap and ready available raw materials used in the preparing process, controllable batch production of nano-grade high-purity Bi, BiOCl, Bi24O31CL10 or Bi2O2.33, reusable electrolyte, high compatibility with the environment.
Description
Technical field
The present invention relates to a kind of synthetic method of bismuth based nano-material, particularly a kind of method from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal.
Background technology
The distinctive surface effects of nano material, small-size effect, quantum effect, macro quanta tunnel effect and dielectric confinement effect, make when nano material has the macroscopic material performance, also have excellent physics, chemical property concurrently, receive much concern at high-technology field.Bismuth manifests unique advantage as a kind of important dopant material at aspects such as light, magnetic, electricity.Wherein, six side's bismuths are good thermoelectric materials under a kind of potential room temperature, and theoretical investigation has foretold that the nanometer bismuth has excellent more thermoelectricity capability; Nanometer bismuth oxychloride is showing excellent performance aspect catalyzed oxidation, mineral dye, the photoluminescence; The bismuth oxide compound is the important raw and processed materials of synthetic at present bismuth-containing oxygen functional materials, and nano level bismuth oxide compound has significant advantage to the raising of performances such as the catalytic performance of complex functionality material, non-linear optical property, superconductivity, oxonium ion transmission performance, ferroelectricity, ferromegnetism.
At present, the method for bismuth based nano-materials such as synthetic bismuth, bismuth oxychloride, bismuth oxide compound mainly contains chemical precipitation method, sol-gel method, solvent thermal synthesis method, anti-microemulsion method, chemical Vapor deposition process (Journal of Solid State Chemistry180 (2007): 2510-2516).In chemical precipitation method, solvent thermal synthesis method, the anti-microemulsion method nano materials process, the industrial pollution of generation is bigger, and production cost is higher, and purity, the size of the chemical precipitation method products therefrom of industrial main employing at present are restricted; Sol-gel method and chemical Vapor deposition process need the high temperature pyrolysis of organic precursor, the building-up process complexity, and equipment is disposable to have high input, and operator are had relatively high expectations.The electrochemical synthesis nano material is that a kind of with low cost, simple to operate, productive rate and purity are higher relatively, is suitable for the desirable preparation method of industrialized mass production.Research by electrochemical synthesis bismuth based compound is more, and has successfully obtained a series of bismuth based compounds.But, the direct bright rare report of research from bismuth metal control electrolytic synthesis nanometer bismuth based compound.
Summary of the invention
The object of the present invention is to provide a kind of with low cost, product purity height, pattern homogeneous, technical process is short, and is simple to operate, production efficiency height, the environment friendly and pollution-free method from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal.
The technical solution that realizes the object of the invention is: a kind of method from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal, at first, NaCl, EDTA are placed container, and add distilled water stirring, dissolving; Then, regulate pH value, make solution be alkalescence dripping NaOH solution in the solution that makes; Then, be electrolytic solution with the mixing solutions that is alkalescence, be anode with the bismuth metal, make target material after the electrolysis; At last, under agitation condition,,, make the ultimate aim nano material being lower than drying under 200 ℃ of temperature with the target material distilled water wash.
The present invention compared with prior art, its remarkable advantage: 1, the present invention is anode material with the bismuth metal, by regulating the ratio of sodium-chlor, EDTA and sodium hydroxide each component in the aqueous solution, can control synthetic a large amount of target product, nanometer Bi, BiOCl, Bi
24O
31Cl
10Or Bi
2O
2.33, output and purity are higher; 2, in the electrolytic process, the complexing of the Bi that produces by EDTA and electrolysis increases bi content in the solution, impels reaction to continue to carry out, and effectively controls Bi ionic concn in the solution, thereby obtain the nano level target product; 3, this electrolytic solution can be reused, and only has hydrogen to discharge in the process, does not have other " three wastes " pollutents, is suitable for industrialized mass production high-purity nm Bi, BiOCl, Bi
24O
31Cl
10Or Bi
2O
2.334, this electrolytic process is raw materials used cheap and easy to get, uniform product appearance, and technical process is short, and is simple to operate.
Description of drawings
Fig. 1 is the electrolytic synthesis process flow sheet of the present invention from the method for the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal.
Fig. 2 is the SEM figure of the present invention from the method synthetic Bi nanometer sheet of the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal.
Fig. 3 is the XRD figure of the present invention from the method synthetic Bi nanometer sheet of the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal.
Fig. 4 is the SEM figure of the present invention from the method synthetic BiOCl nano powder of the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal.
Fig. 5 is the XRD figure of the present invention from the method synthetic BiOCl nano powder of the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal.
Fig. 6 is the method synthetic Bi of the present invention from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal
24O
31Cl
10The SEM figure of nano powder.
Fig. 7 is the method synthetic Bi of the present invention from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal
24O
31Cl
10The XRD figure of nano powder.
Fig. 8 is the method synthetic Bi of the present invention from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal
2O
2.33The SEM figure of nano powder.
Fig. 9 is the method synthetic Bi of the present invention from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal
2O
2.33The XRD figure of nano powder.
Embodiment
The invention discloses a kind of method, it is characterized in that it comprises the steps: from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal
The first step: NaCl, EDTA are placed container, add distilled water and stir, dissolve;
Second step: in the solution that the first step makes, drip NaOH solution and regulate pH value, make solution be alkalescence;
The 3rd step: the mixing solutions that makes with second step is an electrolytic solution, is anode with the bismuth metal, makes target material after the electrolysis;
The 4th step: under the agitation condition,,, make the ultimate aim nano material being lower than drying under 200 ℃ of temperature with the target material distilled water wash.
The proportionlity NaCl amount of substance (mol) of each material that the first step adds: EDTA amount of substance (mol): the volume of distilled water (ml) is (0.005～0.2): (0.002～0.05): 100; The scope of regulating pH value in the 3rd step is PH 〉=7.
As NaCl amount of substance (mol): EDTA amount of substance (mol) is (0.005～0.2): (0.002～0.05), the scope of pH value are 7～9 o'clock, and the ultimate aim nano material that makes is Bi; As NaCl amount of substance (mol): EDTA amount of substance (mol) is (0.005～0.2): (0.002～0.015), the scope of pH value are 9～11 o'clock, and the ultimate aim nano material that makes is BiOCl; As NaCl amount of substance (mol): EDTA amount of substance (mol) is (0.005～0.2): (0.016～0.05), the scope of pH value are 9～11 o'clock, and the ultimate aim nano material that makes is Bi
24O
31Cl
10As NaCl amount of substance (mol): EDTA amount of substance (mol) is (0.005～0.2): (0.002～0.05), the scope of pH value is＞11 o'clock, the ultimate aim nano material that makes is Bi
2O
2.33
Below in conjunction with specific embodiment the present invention is described in further detail.
Get the commercially available analytical pure NaCl of 0.05mol, the commercially available analytical pure EDTA of 0.02mol places beaker, adds that 100ml distilled water stirs, dissolving, further with commercially available analytical pure NaOH prepared NaOH aqueous solution adjusting PH=8.Inserting direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, electrolysis 2h separates out the spongy metal bismuth at negative electrode.Black spongy metal bismuth is taken out, add 20ml distilled water, strong mixing 20min filters, and drying obtains the 0.4472g black powder, and this powder is analyzed through SEM (as shown in Figure 2), XRD (as shown in Figure 3), and this black powder is the Bi nanometer sheet.
Embodiment 2
Continuing to drip with the commercially available analytical pure NaOH prepared NaOH aqueous solution in the electrolytic solution of case 1 to regulate PH=10, insert direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of faint yellow precipitations appear in electrolysis 4h in the solution.Should faint yellow precipitation take out and use the 20ml distilled water wash, and filter, drying obtains the 0.8651g yellow powder, and this powder is analyzed through SEM (as shown in Figure 6), XRD (as shown in Figure 7), and this yellow powder is Bi
24O
31Cl
10Nano powder.
Embodiment 3
The 5mol/L NaOH aqueous solution that continues to drip with commercially available analytical pure NaOH preparation in the electrolytic solution of case 2 is regulated PH=13, inserts direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, voltage is 10V, and a large amount of yellow mercury oxides appear in electrolysis 2h in the solution.This yellow mercury oxide is taken out and use the 20ml distilled water wash, filter, drying obtains the 0.4211g yellow powder, and this powder is analyzed through SEM (as shown in Figure 8), XRD (as shown in Figure 9), and this yellow powder is Bi
2O
2.33Nanometer sheet.
Embodiment 4
Get the commercially available analytical pure NaCl of 0.05mol, the commercially available analytical pure EDTA of 0.005mol places beaker, adds that 100ml distilled water stirs, dissolving, further with commercially available analytical pure NaOH prepared NaOH aqueous solution adjusting PH=8.Inserting direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, electrolysis 3h separates out the spongy metal bismuth at negative electrode.Black spongy metal bismuth is taken out, add 20ml distilled water, strong mixing 1h filters, and drying obtains the 0.6230g black powder, and this powder is analyzed through SEM (as shown in Figure 2), XRD (as shown in Figure 3), and this black powder is the Bi nanometer sheet.
Embodiment 5
Continuing to drip with the commercially available analytical pure NaOH prepared NaOH aqueous solution in the electrolytic solution of case 4 to regulate PH=11, insert direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of white precipitates appear in electrolysis 4h in the solution.This white precipitate is taken out and use the 20ml distilled water wash, filter, drying obtains the 0.8712g white powder, and this powder is analyzed through SEM (as shown in Figure 4), XRD (as shown in Figure 5), and this white powder is the BiOCl nano powder.
Embodiment 6
In the electrolytic solution of case 5, continue to drip to regulate PH=14, stir with the commercially available analytical pure NaOH prepared NaOH aqueous solution.Inserting direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of yellow mercury oxides appear in electrolysis 3h in the solution.This yellow mercury oxide is taken out and use the 20ml distilled water wash, and repeated washing twice or thrice filters, and drying obtains the 3.2416g yellow powder, and this powder is analyzed through SEM (as shown in Figure 8), XRD (as shown in Figure 9), and this yellow powder is Bi
2O
2.33Nanometer sheet.
Embodiment 7
Get the commercially available analytical pure NaCl of 0.005mol, the commercially available analytical pure EDTA of 0.002mol places beaker, adds that 100ml distilled water stirs, dissolving, further with commercially available analytical pure NaOH prepared NaOH aqueous solution adjusting PH=8.Inserting direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, electrolysis 2h separates out the spongy metal bismuth at negative electrode.Black spongy metal bismuth is taken out, add 20ml distilled water, strong mixing 20min filters, and drying obtains the 0.1196g black powder, and this powder is analyzed through SEM (as shown in Figure 2), XRD (as shown in Figure 3), and this black powder is the Bi nanometer sheet.
Embodiment 8
Continuing to drip with the commercially available analytical pure NaOH prepared NaOH aqueous solution in the electrolytic solution of case 7 to regulate PH=11, insert direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of white precipitates appear in electrolysis 4h in the solution.This white precipitate is taken out and use the 20ml distilled water wash, filter, drying obtains the 0.0826g white powder, and this powder is analyzed through SEM (as shown in Figure 4), XRD (as shown in Figure 5), and this white powder is a BiOCl nano powder BiOCl nano powder.
Embodiment 9
Continuing to drip with the commercially available analytical pure NaOH prepared NaOH aqueous solution in the electrolytic solution of case 8 to regulate the PH=11 stirring and dissolving, insert direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, voltage is 10V, and a large amount of yellow mercury oxides appear in electrolysis 3h in the solution.This yellow mercury oxide is taken out and use the 20ml distilled water wash, and repeated washing twice or thrice filters, and drying obtains the 0.3214g yellow powder, and this powder is analyzed through SEM (as shown in Figure 8), XRD (as shown in Figure 9), and this yellow powder is Bi
2O
2.33Nanometer sheet.
Get the commercially available analytical pure NaCl of 0.005mol, the commercially available analytical pure EDTA of 0.016mol places beaker, adds that 100ml distilled water stirs, dissolving, further with commercially available analytical pure NaOH prepared NaOH aqueous solution adjusting PH=8.Inserting direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, electrolysis 2h separates out the spongy metal bismuth at negative electrode.Black spongy metal bismuth is taken out, add 20ml distilled water, strong mixing 20min filters, and drying obtains the 0.1084g black powder, and this powder is analyzed through SEM (as shown in Figure 2), XRD (as shown in Figure 3), and this black powder is the Bi nanometer sheet.
Continuing to drip with the commercially available analytical pure NaOH prepared NaOH aqueous solution in the electrolytic solution of case 10 to regulate PH=11, insert direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of faint yellow precipitations appear in electrolysis 4h in the solution.Should faint yellow precipitation take out and use the 20ml distilled water wash, and filter, drying obtains the 0.0914g yellow powder, and this powder is analyzed through SEM (as shown in Figure 6), XRD (as shown in Figure 7), and this yellow powder is Bi
24O
31Cl
10Nano powder.
The 5mol/LNaOH aqueous solution that continues to drip with commercially available analytical pure NaOH preparation in the electrolytic solution of case 11 is regulated PH=13, inserts direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, voltage is 10V, and a large amount of yellow mercury oxides appear in electrolysis 3h in the solution.This yellow mercury oxide is taken out and use the 20ml distilled water wash, and repeated washing twice or thrice filters, and drying obtains the 0.2765g yellow powder, and this powder is analyzed through SEM (as shown in Figure 8), XRD (as shown in Figure 9), and this yellow powder is Bi
2O
2.33Nanometer sheet.
Embodiment 13
Get the commercially available analytical pure NaCl of 0.2mol, the commercially available analytical pure EDTA of 0.015mol places beaker, adds that 100ml distilled water stirs, dissolving, further with commercially available analytical pure NaOH prepared NaOH aqueous solution adjusting PH=8.Inserting direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, electrolysis 2h separates out the spongy metal bismuth at negative electrode.Black spongy metal bismuth is taken out, add 20ml distilled water, strong mixing 20min filters, and drying obtains the 0.0643g black powder, and this powder is analyzed through SEM (as shown in Figure 2), XRD (as shown in Figure 3), and this black powder is the Bi nanometer sheet.
Embodiment 14
Continuing to drip with the commercially available analytical pure NaOH prepared NaOH aqueous solution in the electrolytic solution of case 13 to regulate PH=9, insert direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of white precipitates appear in electrolysis 4h in the solution.This white precipitate is taken out and use the 20ml distilled water wash, filter, drying obtains the 0.0437g white powder, and this powder is analyzed through SEM (as shown in Figure 4), XRD (as shown in Figure 5), and this white powder is the BiOCl nano powder.
Embodiment 15
Continuing to drip with the commercially available analytical pure NaOH prepared NaOH aqueous solution in the electrolytic solution of case 14 to regulate PH=13, insert direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of yellow mercury oxides appear in electrolysis 3h in the solution.This yellow mercury oxide is taken out and use the 20ml distilled water wash, and repeated washing twice or thrice filters, and drying obtains the 0.2177g yellow powder, and this powder is analyzed through SEM (as shown in Figure 8), XRD (as shown in Figure 9), and this yellow powder is Bi
2O
2.33Nanometer sheet.
Get the commercially available analytical pure NaCl of 0.2mol, the commercially available analytical pure EDTA of 0.05mol places beaker, adds that 100ml distilled water stirs, dissolving, further with the 5mol/L NaOH aqueous solution adjusting PH=8 of commercially available analytical pure NaOH preparation.Inserting direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, electrolysis 2h separates out the spongy metal bismuth at negative electrode.Black spongy metal bismuth is taken out, add 20ml distilled water, strong mixing 20min filters, and drying obtains the 0.1304g black powder, and this powder is analyzed through SEM (as shown in Figure 2), XRD (as shown in Figure 3), and this black powder is the Bi nanometer sheet.
Embodiment 17
Continuing to drip with the commercially available analytical pure NaOH prepared NaOH aqueous solution in the electrolytic solution of case 16 to regulate PH=9, insert direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of faint yellow precipitations appear in electrolysis 4h in the solution.Should faint yellow precipitation take out and use the 20ml distilled water wash, and filter, drying obtains the 0.0844g yellow powder, and this powder is analyzed through SEM (as shown in Figure 6), XRD (as shown in Figure 7), and this yellow powder is Bi
24O
31Cl
10Nano powder.
Embodiment 18
Continuing to drip with the commercially available analytical pure NaOH prepared NaOH aqueous solution in the electrolytic solution of case 17 to regulate PH=13, insert direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of yellow mercury oxides appear in electrolysis 3h in the solution.This yellow mercury oxide is taken out and use the 20ml distilled water wash, and repeated washing twice or thrice filters, and drying obtains the 0.4117g yellow powder, and this powder is analyzed through SEM (as shown in Figure 8), XRD (as shown in Figure 9), and this yellow powder is Bi
2O
2.33Nanometer sheet.
Embodiment 19
Get the commercially available analytical pure NaCl of 0.05mol, the commercially available analytical pure EDTA of 0.02mol places beaker, adding 100ml distilled water stirs, dissolves, further add the 5mol/l.NaOH 20ml solution with commercially available analytical pure NaOH preparation, the pH value of mixing solutions is much larger than 11.Inserting direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of yellow mercury oxides appear in electrolysis 3h in the solution.This yellow mercury oxide is taken out and use the 20ml distilled water wash, and repeated washing twice or thrice filters, and drying obtains the 4.2115g yellow powder, and this powder is analyzed through SEM (as shown in Figure 8), XRD (as shown in Figure 9), and this yellow powder is Bi
2O
2.33Nanometer sheet.
Get the commercially available analytical pure NaCl of 0.005mol, the commercially available analytical pure EDTA of 0.002mol, place beaker, add 100ml distilled water and stir, dissolve, further add the 10mol/l.NaOH 20ml solution with commercially available analytical pure NaOH preparation, the pH value of mixing solutions is much larger than 11.Inserting direct supply, is the anodic corrosion electrode with the bismuth metal, logical direct current, and voltage is 10V, a large amount of yellow mercury oxides appear in electrolysis 2h in the solution.This yellow mercury oxide is taken out and use the 20ml distilled water wash, and repeated washing twice or thrice filters, and drying obtains the 0.2457g yellow powder, and this powder is analyzed through SEM (as shown in Figure 8), XRD (as shown in Figure 9), and this yellow powder is Bi
2O
2.33Nanometer sheet.
Claims (7)
1. the method from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal is characterized in that it comprises the steps:
The first step: NaCl, EDTA are placed container, add distilled water and stir, dissolve;
Second step: in the solution that the first step makes, drip NaOH solution and regulate pH value, make solution be alkalescence;
The 3rd step: the mixing solutions that makes with second step is an electrolytic solution, is anode with the bismuth metal, makes target material after the electrolysis;
The 4th step: under the agitation condition,,, make the ultimate aim nano material being lower than drying under 200 ℃ of temperature with the target material distilled water wash.
2. the method from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal according to claim 1, it is characterized in that the proportionlity NaCl amount of substance (mol) of each material that the first step adds: EDTA amount of substance (mol): the volume of distilled water (ml) is (0.005～0.2): (0.002～0.05): 100.
3. the method from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal according to claim 1, it is characterized in that: the scope of regulating pH value in the 3rd step is PH 〉=7.
4. according to claim 1,2 or 3 described methods from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal, it is characterized in that: as NaCl amount of substance (mol): EDTA amount of substance (mol) is (0.005～0.2): (0.002～0.05), the scope of pH value is 7～9 o'clock, and making the ultimate aim nano material is Bi.
5. according to claim 1,2 or 3 described methods from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal, it is characterized in that working as: as NaCl amount of substance (mol): EDTA amount of substance (mol) is (0.005～0.2): (0.002～0.015), the scope of pH value is 9～11 o'clock, and making the ultimate aim nano material is BiOCl.
6. according to claim 1,2 or 3 described methods from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal, it is characterized in that: as NaCl amount of substance (mol): EDTA amount of substance (mol) is (0.005～0.2): (0.016～0.05), the scope of pH value is 9～11 o'clock, and making the ultimate aim nano material is Bi
24O
31Cl
10
7. according to claim 1,2 or 3 described methods from the synthetic bismuth based nano-material of the direct electrolysis control of bismuth metal, it is characterized in that: as NaCl amount of substance (mol): EDTA amount of substance (mol) is (0.005～0.2): (0.002～0.05), the scope of pH value is＞11 o'clock, and making the ultimate aim nano material is Bi
2O
2.33
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| CN103785426A (en) * | 2014-01-09 | 2014-05-14 | 河北科技大学 | BiOCl base heterojunction with visible-light catalytic activity and preparation method thereof |
| RU2545342C2 (en) * | 2013-04-12 | 2015-03-27 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Юго-Западный государственный университет" (ЮЗГУ) | Method of producing bismuth nanoparticles |
| CN105060341A (en) * | 2015-08-06 | 2015-11-18 | 中国科学院合肥物质科学研究院 | Micro-nano structure bismuth oxide material and preparation method thereof |
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| CN100584763C (en) * | 2006-11-10 | 2010-01-27 | 宝山钢铁股份有限公司 | Method for preparing nano bismuth oxide |
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| CN111530481A (en) * | 2020-05-26 | 2020-08-14 | 广东石油化工学院 | Method for rapidly preparing BiOBr nanosheet |
| CN114669308A (en) * | 2022-04-01 | 2022-06-28 | 哈尔滨理工大学 | BiOCl/Bi preparation by means of electrochemical method in-situ reaction24O31Cl10Method for compounding powder |
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