CN106335873A - Method for preparing Pb3(PO4)2 nanowire film - Google Patents
Method for preparing Pb3(PO4)2 nanowire film Download PDFInfo
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- CN106335873A CN106335873A CN201610940877.8A CN201610940877A CN106335873A CN 106335873 A CN106335873 A CN 106335873A CN 201610940877 A CN201610940877 A CN 201610940877A CN 106335873 A CN106335873 A CN 106335873A
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- pbs
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- thin film
- deposition
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- 239000002070 nanowire Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910000156 lead(II) phosphate Inorganic materials 0.000 title abstract 4
- 239000007853 buffer solution Substances 0.000 claims abstract description 14
- 238000000151 deposition Methods 0.000 claims abstract description 6
- 230000008021 deposition Effects 0.000 claims abstract description 5
- 239000010409 thin film Substances 0.000 claims description 21
- 238000004070 electrodeposition Methods 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- 239000010408 film Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 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 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000002484 cyclic voltammetry Methods 0.000 claims description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical group [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000007772 electrode material Substances 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000004014 plasticizer Substances 0.000 abstract description 2
- -1 sensors Substances 0.000 abstract 1
- HUTDDBSSHVOYJR-UHFFFAOYSA-H bis[(2-oxo-1,3,2$l^{5},4$l^{2}-dioxaphosphaplumbetan-2-yl)oxy]lead Chemical compound [Pb+2].[Pb+2].[Pb+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O HUTDDBSSHVOYJR-UHFFFAOYSA-H 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0009—Forming specific nanostructures
- B82B3/0038—Manufacturing processes for forming specific nanostructures not provided for in groups B82B3/0014 - B82B3/0033
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a method for preparing a Pb3(PO4)2 nanowire film. The method comprises the following steps: depositing PbS on the surface of an electrode by using an electric deposition way to form a carrier film, immersing the electrode in a PBS buffer solution, growing for 48 to 72 hours in a constant-temperature water-bath pot, and finally taking out the electrode, wherein the Pb3(PO4)2 nanowire film spontaneously grows on the electrode. The method is simple in preparation process; and the prepared Pb3(PO4)2 nanowire film is large in adhesive force, regular in shape, large in length-diameter ratio, homogenous in diameter, high in efficiency, low in cost and easy in mass production and has potential application value in the fields such as electrode materials, sensors, plasticizers and the like.
Description
Technical field
The invention belongs to nano film material field, prepare pb particularly to one kind3(po4)2The method of nano wire film.
Background technology
pb3(po4)2It is often hexagon colourless crystallization or white powder, water insoluble and alcohol, it is dissolved in nitric acid it is impossible to burn,
Slowly hydrolyze in hot water, be a kind of important inorganic salt product, industrial be commonly used for electrode material and stabilizer for plastics, simultaneously
It is one of best ferroelasticity compound of generally acknowledging at present.At present, main production process both domestic and external is as follows: in room temperature condition
Under, with plumbi nitrass and sodium phosphate etc. as raw material, direct precipitation method one-step synthesis lead phosphate in aqueous.Above-mentioned method produces
Lead phosphate purity out is low, impurity content is high, particle diameter is uneven, pattern is irregular it is impossible to it is brilliant to lead phosphate to meet modern industry
The requirement of whisker material.Using chemical bath on pbs thin film autonomous growth pb3(po4)2Nano wire, method is simple, compares
In other growing methods, in addition its great advantage exactly need not add reducing agent, and preparation process is simple, and nano wire pattern rule
Whole, draw ratio is big, and diameter is homogeneous, suitable large-scale production.
Content of the invention
It is an object of the invention to provide one kind prepares pb3(po4)2The method of nano wire film.
The principle of the present invention and thinking: pbs is deposited on electrode surface by the method using electro-deposition, forms a kind of carrier thin
Film, immerses electrode in pbs buffer solution, then grows in thermostat water bath 48 ~ 72 hours, finally takes out electrode, on electrode
Just spontaneously grow upper pb3(po4)2Nano wire film.
Concretely comprise the following steps:
(1) by the conductive glass electrode cutting out in advance respectively with analysis pure acetone, analysis straight alcohol and each ultrasonic cleaning 3 of secondary water
Min, air is obtained base electrode after being dried.
(2) measure the pb (no that 1ml concentration is 0.2 mol/l successively3)2Solution, 1 ml concentration are the edta of 0.2 mol/l
Solution, 3.5 ml concentration are the na of 0.3 mol/l2s2o3Solution and the na that 4 ml concentration are 1.25 mol/l2so4Solution is put together
Mix homogeneously in 20 ml beakers, prepared electro-deposition pbs thin film bottom liquid.
(3) set up three-electrode system in the electro-deposition pbs thin film bottom liquid that step (2) is obtained, wherein, step (1) is obtained
Base electrode as working electrode, ag/agcl is reference electrode, and pt is auxiliary electrode, carries out electro-deposition with cyclic voltammetry,
Sweep limitss are -1 ~ 0v, and scanning speed is 0.05v/s, and scanning hop count is 50 ~ 60 sections, after deposition terminates, take out working electrode,
Pbs thin film, prepared pbs base electrode are just deposited on its surface.
(4) measure 8ml pbs buffer solution to add in clean growth bottle, the pbs matrix electricity then prepared by step (3)
Extremely tiltedly put in growth bottle, then growth bottle is placed in reaction 48 ~ 72 hours under constant temperature in 45 DEG C of water-bath, finally take out
Pbs base electrode, the thin film growing thereon is pb3(po4)2Nano wire film.
Described conductive glass electrode is indium-tin oxide electrode.
Described pbs buffer solution is the na that concentration is 0.2mol/l2hpo4-nah2po4Buffer solution, its ph=6.8.
The inventive method preparation process is simple, and obtained pb3(po4)2The adhesive force of nano wire film is strong, and pattern is advised
Whole, draw ratio is big, and diameter is homogeneous, efficiency high, low cost it is easy to large-scale production, in electrode material, sensor and plasticizer etc.
There is potential using value in field.
Brief description
Fig. 1 is the pb being obtained in the embodiment of the present invention 13(po4)2The X-ray diffraction pattern of nano wire.
Fig. 2 is the scanning electron microscope (SEM) photograph of the pbs thin film being obtained in the embodiment of the present invention 1.
Fig. 3 is the pb being obtained in the embodiment of the present invention 13(po4)2The scanning electron microscope (SEM) photograph of nano wire film.
Specific embodiment
Below with reference to Figure of description and specific embodiment, the present invention is described in further details.
Embodiment 1:
(1) by the conductive glass electrode cutting out in advance respectively with analysis pure acetone, analysis straight alcohol and each ultrasonic cleaning 3 of secondary water
Min, air is obtained base electrode after being dried.
(2) measure the pb (no that 1ml concentration is 0.2 mol/l successively3)2Solution, 1 ml concentration are the edta of 0.2 mol/l
Solution, 3.5 ml concentration are the na of 0.3 mol/l2s2o3Solution and the na that 4 ml concentration are 1.25 mol/l2so4Solution is put together
Mix homogeneously in 20 ml beakers, prepared electro-deposition pbs thin film bottom liquid.
(3) set up three-electrode system in the electro-deposition pbs thin film bottom liquid that step (2) is obtained, wherein, step (1) is obtained
Base electrode as working electrode, ag/agcl is reference electrode, and pt is auxiliary electrode, carries out electro-deposition with cyclic voltammetry,
Sweep limitss are -1 ~ 0v, and scanning speed is 0.05v/s, and scanning hop count is 50 sections, after deposition terminates, take out working electrode, its table
Pbs thin film, prepared pbs base electrode are just deposited on face.
(4) measure 8ml pbs buffer solution to add in clean growth bottle, the pbs matrix electricity then prepared by step (3)
Extremely tiltedly put in growth bottle, then growth bottle is placed in reaction 48 hours under constant temperature in 45 DEG C of water-bath, finally take out pbs
Base electrode, the thin film growing thereon is pb3(po4)2Nano wire film.
Described conductive glass electrode is indium-tin oxide electrode.
Described pbs buffer solution is the na that concentration is 0.2mol/l2hpo4-nah2po4Buffer solution, its ph=6.8.
Fig. 1 is the X-ray diffraction pattern of the present embodiment products therefrom, and as seen from Figure 1, the product that base electrode is obtained is
pb3(po4)2Nano wire film.Fig. 2 is the scanning electron microscope (SEM) photograph of the pbs thin film of electro-deposition preparation in the present embodiment, is clearly seen by Fig. 2
Granule-morphology to pbs deposit.Fig. 3 is to grow pb on the pbs thin film of electro-deposition in the present embodiment3(po4)2Nano wire is thin
The scanning electron microscope (SEM) photograph of film, by can be clearly apparent pb in Fig. 33(po4)2Nano wire.
Embodiment 2:
(1) by the conductive glass electrode cutting out in advance respectively with analysis pure acetone, analysis straight alcohol and each ultrasonic cleaning 3 of secondary water
Min, air is obtained base electrode after being dried.
(2) measure the pb (no that 1ml concentration is 0.2 mol/l successively3)2Solution, 1 ml concentration are the edta of 0.2 mol/l
Solution, 3.5 ml concentration are the na of 0.3 mol/l2s2o3Solution and the na that 4 ml concentration are 1.25 mol/l2so4Solution is put together
Mix homogeneously in 20 ml beakers, prepared electro-deposition pbs thin film bottom liquid.
(3) set up three-electrode system in the electro-deposition pbs thin film bottom liquid that step (2) is obtained, wherein, step (1) is obtained
Base electrode as working electrode, ag/agcl is reference electrode, and pt is auxiliary electrode, carries out electro-deposition with cyclic voltammetry,
Sweep limitss are -1 ~ 0v, and scanning speed is 0.05v/s, and scanning hop count is 60 sections, after deposition terminates, take out working electrode, its table
Pbs thin film, prepared pbs base electrode are just deposited on face.
(4) measure 8ml pbs buffer solution to add in clean growth bottle, the pbs matrix electricity then prepared by step (3)
Extremely tiltedly put in growth bottle, then growth bottle is placed in reaction 72 hours under constant temperature in 45 DEG C of water-bath, finally take out pbs
Base electrode, the thin film growing thereon is pb3(po4)2Nano wire film.
Described conductive glass electrode is indium-tin oxide electrode.
Described pbs buffer solution is the na that concentration is 0.2mol/l2hpo4-nah2po4Buffer solution, its ph=6.8.
The above is only the preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment,
All within the scope of the present invention with the various process programs of present inventive concept no substantial differences.
Claims (1)
1. one kind prepares pb3(po4)2The method of nano wire film is it is characterised in that concretely comprise the following steps:
(1) by the conductive glass electrode cutting out in advance respectively with analysis pure acetone, analysis straight alcohol and each ultrasonic cleaning 3 of secondary water
Min, air is obtained base electrode after being dried；
(2) measure the pb (no that 1ml concentration is 0.2 mol/l successively3)2Solution, 1 ml concentration are that the edta of 0.2 mol/l is molten
Liquid, 3.5 ml concentration are the na of 0.3 mol/l2s2o3Solution and the na that 4 ml concentration are 1.25 mol/l2so4Solution is placed in together
Mix homogeneously in 20 ml beakers, prepared electro-deposition pbs thin film bottom liquid；
(3) set up three-electrode system in the electro-deposition pbs thin film bottom liquid that step (2) is obtained, wherein, the base that step (1) is obtained
As working electrode, ag/agcl is reference electrode to body electrode, and pt is auxiliary electrode, carries out electro-deposition with cyclic voltammetry, scanning
Scope is -1 ~ 0v, and scanning speed is 0.05v/s, and scanning hop count is 50 ~ 60 sections, after deposition terminates, takes out working electrode, its table
Pbs thin film, prepared pbs base electrode are just deposited on face；
(4) measure 8ml pbs buffer solution to add in clean growth bottle, the pbs base electrode then prepared by step (3) is oblique
Put in growth bottle, then growth bottle is placed in reaction 48 ~ 72 hours under constant temperature in 45 DEG C of water-bath, finally take out pbs
Base electrode, the thin film growing thereon is pb3(po4)2Nano wire film；
Described conductive glass electrode is indium-tin oxide electrode；
Described pbs buffer solution is the na that concentration is 0.2mol/l2hpo4-nah2po4Buffer solution, its ph=6.8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610940877.8A CN106335873B (en) | 2016-10-26 | 2016-10-26 | The method that one kind prepares 2 nano wire films of Pb3 (PO4) |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610940877.8A CN106335873B (en) | 2016-10-26 | 2016-10-26 | The method that one kind prepares 2 nano wire films of Pb3 (PO4) |
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| Publication Number | Publication Date |
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| CN106335873A true CN106335873A (en) | 2017-01-18 |
| CN106335873B CN106335873B (en) | 2018-04-13 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110231378A (en) * | 2019-05-23 | 2019-09-13 | 桂林理工大学 | A kind of preparation method of super-hydrophobic gold electrode |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054266A (en) * | 2007-05-30 | 2007-10-17 | 北京科技大学 | Method of preparing photoelectrocatalysis material zinc ferrite film from lead-zinc tailings |
| CN105499596A (en) * | 2015-12-06 | 2016-04-20 | 桂林理工大学 | Method for spontaneously growing Au nanometer particles on electro-deposited CdSe film |
-
2016
- 2016-10-26 CN CN201610940877.8A patent/CN106335873B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054266A (en) * | 2007-05-30 | 2007-10-17 | 北京科技大学 | Method of preparing photoelectrocatalysis material zinc ferrite film from lead-zinc tailings |
| CN105499596A (en) * | 2015-12-06 | 2016-04-20 | 桂林理工大学 | Method for spontaneously growing Au nanometer particles on electro-deposited CdSe film |
Non-Patent Citations (1)
| Title |
|---|
| HONGCHENG PAN ET AL.: "Spontaneous Growth of Au Nanoparticles onto CdS, ZnS or PbS Thin Films for Electrochemical Immunosensors", 《INT.J.ELECTROCHEM.SCI.》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110231378A (en) * | 2019-05-23 | 2019-09-13 | 桂林理工大学 | A kind of preparation method of super-hydrophobic gold electrode |
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| CN106335873B (en) | 2018-04-13 |
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Application publication date: 20170118 Assignee: URIT Medical Electronic Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980044242 Denomination of invention: A Method for Preparing Pb3 (PO4) 2 Nanowire Thin Films Granted publication date: 20180413 License type: Common License Record date: 20231024 |