CN106335873B - The method that one kind prepares 2 nano wire films of Pb3 (PO4) - Google Patents
The method that one kind prepares 2 nano wire films of Pb3 (PO4) Download PDFInfo
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- CN106335873B CN106335873B CN201610940877.8A CN201610940877A CN106335873B CN 106335873 B CN106335873 B CN 106335873B CN 201610940877 A CN201610940877 A CN 201610940877A CN 106335873 B CN106335873 B CN 106335873B
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- 239000002070 nanowire Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000004070 electrodeposition Methods 0.000 claims abstract description 20
- 239000007853 buffer solution Substances 0.000 claims abstract description 14
- 229910000156 lead(II) phosphate Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 15
- 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910000162 sodium phosphate Inorganic materials 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
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000002484 cyclic voltammetry Methods 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical group [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 claims description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 4
- 239000007772 electrode material Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 239000004014 plasticizer Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 abstract 3
- 239000010409 thin film Substances 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 9
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 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
- 238000002604 ultrasonography Methods 0.000 description 3
- 238000004519 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
- 238000011031 large-scale manufacturing process Methods 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
- 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 one kind to prepare Pb3(PO4)2The method of nano wire film.PbS is deposited on electrode surface using the method for electro-deposition, forms a kind of carrier thin film, electrode is immersed in PBS buffer solutions, then when growth 48 ~ 72 is small in thermostat water bath, finally takes out electrode, upper Pb is just spontaneously grown on electrode3(PO4)2Nano wire film.The method of the present invention preparation process is simple, and obtained Pb3(PO4)2The strong adhesive force of nano wire film, regular appearance, draw ratio is big, and diameter is homogeneous, efficient, and cost is low, is easy to mass produce, and has potential application value in fields such as electrode material, sensor and plasticizer.
Description
Technical field
The invention belongs to nano film material field, more particularly to one kind prepares Pb3(PO4)2The method of nano wire film.
Background technology
Pb3(PO4)2Often it is hexagon colourless crystallization or white powder, not soluble in water and alcohol, is dissolved in nitric acid, it is impossible to burn,
Slowly hydrolyzed in hot water, be a kind of important inorganic salt product, be industrially commonly used for electrode material and stabilizer for plastics, while
It is one of best ferroelasticity compound generally acknowledged at present.At present, main production process both domestic and external is as follows：In room temperature condition
Under, with plumbi nitras and sodium phosphate etc. for raw material, direct precipitation method one-step synthesis lead phosphate in aqueous.Above-mentioned method production
Lead phosphate purity out is low, impurity content is high, particle diameter is uneven, pattern is irregular, it is impossible to meets that modern industry is brilliant to lead phosphate
The requirement of whisker material.Using chemical bath in PbS film autonomous growth Pb3(PO4)2Nano wire, method is simple and practicable, compares
In other growing methods, for its great advantage exactly without in addition adding reducing agent, preparation process is simple, and nano wire pattern is advised
Whole, draw ratio is big, and diameter is homogeneous, is adapted to large-scale production.
The content of the invention
The object of the present invention is to provide one kind to prepare Pb3(PO4)2The method of nano wire film.
The principle of the present invention and thinking：PbS is deposited on electrode surface using the method for electro-deposition, it is thin to form a kind of carrier
Film, electrode is immersed in PBS buffer solutions, then when growth 48 ~ 72 is small in thermostat water bath, electrode is finally taken out, on electrode
Just spontaneously grow upper Pb3(PO4)2Nano wire film.
Concretely comprise the following steps：
(1) by the conductive glass electrode cut out in advance respectively with analysis pure acetone, analysis straight alcohol and each ultrasound of secondary water
3 min are cleaned, base electrode is made after being air-dried.
(2) Pb (NO that 1mL concentration is 0.2 mol/L are measured successively3)2Solution, the EDTA that 1 mL concentration is 0.2 mol/L
Solution, the Na that 3.5 mL concentration are 0.3 mol/L2S2O3Solution and the Na that 4 mL concentration are 1.25 mol/L2SO4Solution is put together
It is uniformly mixed in 20 mL beakers, electro-deposition PbS film bottom liquid is made.
(3) three-electrode system is established in electro-deposition PbS film bottom liquid made from step (2), wherein, step (1) is made
Base electrode as working electrode, Ag/AgCl is reference electrode, and Pt is auxiliary electrode, and electro-deposition is carried out with cyclic voltammetry,
Scanning range is -1 ~ 0V, sweep speed 0.05V/s, and scanning hop count is 50 ~ 60 sections, after deposition, takes out working electrode,
PbS film is just deposited on its surface, PbS base electrodes are made.
(4) measure 8mL PBS buffer solutions to add in clean growth bottle, the PbS matrixes electricity for then preparing step (3)
Extremely tiltedly be put into growth bottle, then will growth bottle be placed in 45 DEG C of water-bath under constant temperature reaction 48 ~ 72 it is small when, finally take out
PbS base electrodes, the film grown thereon are Pb3(PO4)2Nano wire film.
The conductive glass electrode is indium-tin oxide electrode.
The PBS buffer solutions are the Na that concentration is 0.2mol/L2HPO4-NaH2PO4Buffer solution, its pH=6.8.
The method of the present invention preparation process is simple, and obtained Pb3(PO4)2The strong adhesive force of nano wire film, pattern rule
Whole, draw ratio is big, and diameter is homogeneous, efficient, and cost is low, is easy to mass produce, in electrode material, sensor and plasticizer etc.
There is potential application value in field.
Brief description of the drawings
Fig. 1 is obtained Pb in the embodiment of the present invention 13(PO4)2The X-ray diffractogram of nano wire.
Fig. 2 is the scanning electron microscope (SEM) photograph of obtained PbS film in the embodiment of the present invention 1.
Fig. 3 is obtained Pb in the embodiment of the present invention 13(PO4)2The scanning electron microscope (SEM) photograph of nano wire film.
Embodiment
The present invention is described in further details below with reference to Figure of description and specific embodiment.
Embodiment 1：
(1) by the conductive glass electrode cut out in advance respectively with analysis pure acetone, analysis straight alcohol and each ultrasound of secondary water
3 min are cleaned, base electrode is made after being air-dried.
(2) Pb (NO that 1mL concentration is 0.2 mol/L are measured successively3)2Solution, the EDTA that 1 mL concentration is 0.2 mol/L
Solution, the Na that 3.5 mL concentration are 0.3 mol/L2S2O3Solution and the Na that 4 mL concentration are 1.25 mol/L2SO4Solution is put together
It is uniformly mixed in 20 mL beakers, electro-deposition PbS film bottom liquid is made.
(3) three-electrode system is established in electro-deposition PbS film bottom liquid made from step (2), wherein, step (1) is made
Base electrode as working electrode, Ag/AgCl is reference electrode, and Pt is auxiliary electrode, and electro-deposition is carried out with cyclic voltammetry,
Scanning range is -1 ~ 0V, sweep speed 0.05V/s, and scanning hop count is 50 sections, after deposition, takes out working electrode, its table
PbS film is just deposited on face, PbS base electrodes are made.
(4) measure 8mL PBS buffer solutions to add in clean growth bottle, the PbS matrixes electricity for then preparing step (3)
Extremely tiltedly be put into growth bottle, then will growth bottle be placed in 45 DEG C of water-bath under constant temperature reaction 48 it is small when, finally take out PbS
Base electrode, the film grown thereon are Pb3(PO4)2Nano wire film.
The conductive glass electrode is indium-tin oxide electrode.
The PBS buffer solutions are the Na that concentration is 0.2mol/L2HPO4-NaH2PO4Buffer solution, its pH=6.8.
Fig. 1 is the X-ray diffractogram of the present embodiment products therefrom, and as seen from Figure 1, the resulting product is on base electrode
Pb3(PO4)2Nano wire film.Fig. 2 is the scanning electron microscope (SEM) photograph of PbS film prepared by electro-deposition in the present embodiment, is clearly seen by Fig. 2
To the granule-morphology of PbS deposits.Fig. 3 is to grow Pb in the PbS film of electro-deposition in the present embodiment3(PO4)2Nano wire is thin
The scanning electron microscope (SEM) photograph of film, by Pb can be clearly apparent in Fig. 33(PO4)2Nano wire.
Embodiment 2：
(1) by the conductive glass electrode cut out in advance respectively with analysis pure acetone, analysis straight alcohol and each ultrasound of secondary water
3 min are cleaned, base electrode is made after being air-dried.
(2) Pb (NO that 1mL concentration is 0.2 mol/L are measured successively3)2Solution, the EDTA that 1 mL concentration is 0.2 mol/L
Solution, the Na that 3.5 mL concentration are 0.3 mol/L2S2O3Solution and the Na that 4 mL concentration are 1.25 mol/L2SO4Solution is put together
It is uniformly mixed in 20 mL beakers, electro-deposition PbS film bottom liquid is made.
(3) three-electrode system is established in electro-deposition PbS film bottom liquid made from step (2), wherein, step (1) is made
Base electrode as working electrode, Ag/AgCl is reference electrode, and Pt is auxiliary electrode, and electro-deposition is carried out with cyclic voltammetry,
Scanning range is -1 ~ 0V, sweep speed 0.05V/s, and scanning hop count is 60 sections, after deposition, takes out working electrode, its table
PbS film is just deposited on face, PbS base electrodes are made.
(4) measure 8mL PBS buffer solutions to add in clean growth bottle, the PbS matrixes electricity for then preparing step (3)
Extremely tiltedly be put into growth bottle, then will growth bottle be placed in 45 DEG C of water-bath under constant temperature reaction 72 it is small when, finally take out PbS
Base electrode, the film grown thereon are Pb3(PO4)2Nano wire film.
The conductive glass electrode is indium-tin oxide electrode.
The PBS buffer solutions are 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,
It is within the scope of the present invention with various process programs of the present inventive concept without substantial differences.
Claims (1)
1. one kind prepares Pb3(PO4)2The method of nano wire film, it is characterised in that concretely comprise the following steps：
(1) conductive glass electrode cut out in advance is respectively cleaned by ultrasonic 3 with analysis pure acetone, analysis straight alcohol and secondary water respectively
Min, is made base electrode after being air-dried；
(2) Pb (NO that 1mL concentration is 0.2 mol/L are measured successively3)2Solution, the EDTA that 1 mL concentration is 0.2 mol/L are molten
Liquid, the Na that 3.5 mL concentration are 0.3 mol/L2S2O3Solution and the Na that 4 mL concentration are 1.25 mol/L2SO4Solution is placed in together
It is uniformly mixed in 20 mL beakers, electro-deposition PbS film bottom liquid is made；
(3) three-electrode system is established in electro-deposition PbS film bottom liquid made from step (2), wherein, base made from step (1)
For body electrode as working electrode, Ag/AgCl is reference electrode, and Pt is auxiliary electrode, and electro-deposition is carried out with cyclic voltammetry, scanning
Scope is -1 ~ 0V, sweep speed 0.05V/s, and scanning hop count is 50 ~ 60 sections, after deposition, takes out working electrode, its table
PbS film is just deposited on face, PbS base electrodes are made；
(4) measure 8mL PBS buffer solutions to add in clean growth bottle, the PbS base electrodes for then preparing step (3) are oblique
Be put into growth bottle, then will growth bottle be placed in 45 DEG C of water-bath under constant temperature reaction 48 ~ 72 it is small when, finally take out PbS
Base electrode, the film grown thereon are Pb3(PO4)2Nano wire film；
The conductive glass electrode is indium-tin oxide electrode；
The PBS buffer solutions are the Na that concentration is 0.2mol/L2HPO4-NaH2PO4Buffer solution, its pH=6.8.
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| 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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| CN106335873B true CN106335873B (en) | 2018-04-13 |
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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 |
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- 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 |
|---|
| Spontaneous Growth of Au Nanoparticles onto CdS, ZnS or PbS Thin Films for Electrochemical Immunosensors;Hongcheng Pan et al.;《Int.J.Electrochem.Sci.》;20160401;第11卷;第3364-3375页 * |
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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 |