CN109234681A - A method of preparing orderly gold nano cap array - Google Patents
A method of preparing orderly gold nano cap array Download PDFInfo
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- CN109234681A CN109234681A CN201811115626.1A CN201811115626A CN109234681A CN 109234681 A CN109234681 A CN 109234681A CN 201811115626 A CN201811115626 A CN 201811115626A CN 109234681 A CN109234681 A CN 109234681A
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
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- C23C28/345—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates with at least one oxide layer
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- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/10—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing organic acids
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- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
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Abstract
The invention discloses a kind of methods for preparing orderly gold nano cap array, steps are as follows: high-purity aluminum foil is placed in acetone ultrasound to remove surface and oil contaminant, it is subsequently placed in ethyl alcohol and perchloric acid mixed solution and carries out electrochemical polish, after deionized water is rinsed and is dried with nitrogen, the aluminium foil that surface is in smooth mirror surface is obtained；Aluminium foil after polishing is placed in oxalic acid solution, carries out anodic oxidation at a dc voltage, temperature maintains 6-8 DEG C, and sample is then placed in 3-4h in chromic acid and the isometric mixed solution of phosphoric acid, then carries out anodic oxidation again, obtains the PAA template of high-sequential；By sample be placed in saturation copper chloride solution in remove aluminium substrate, the barrier layer of PAA is exposed, using electron beam evaporation deposition machine by gold be deposited on PAA barrier layer surface to get.The orderly gold nano cap array of this method preparation has strongest SERS signal reinforcing effect to CV molecule, is expected to be applied to the trace detection of forbidden drug in aquatic products.
Description
Technical field
The present invention relates to a kind of methods for preparing orderly gold nano cap array.
Background technique
In recent years, Safety of Aquatic Products problem caused by violated antibacterials are abused is increasingly significant.It is remaining anti-in aquatic products
Mushroom drug can not only make pathogen generate drug resistance, but also part antibacterials itself have the side effects such as carcinogenic, mutagenesis.
It is especially the triphen first of representative with crystal violet (crystal violet, CV) and malachite green (malachite green, MG)
Alkanes dyestuff is widely used in culture fishery because cheap and having good sterilizing effect, they are to certainly
Right environment and human health, which are constituted, greatly to threaten.Currently, reliable detection technique more mature to the substance is main
Including spectrophotometry, high performance liquid chromatography (HPLC), Liquid Chromatography/Mass Spectrometry (LC-MS) etc..However, these technologies are mostly based on
The fixed detecting devices of large size, that there are equipment is heavy, expensive, analysis time is long, detects the disadvantages of type is single, and often
Need the pre-processing process of the complexity such as Solid Phase Extraction.
Surface enhanced Raman scattering (surface-enhanced Raman scattering, SERS) technology is because having spirit
Sensitivity is high, and rapidly, detection range is wide, can directly carry out high-resolution finger to gas, liquid and solid for signal response
Line formula identification etc. the incomparable many advantages of traditional technologies and be concerned.SERS technical requirements are used for the change of Molecular Detection
, biosensor material have wide responding range and uniform and stable response signal, thus grinding in terms of substrate
Study carefully one of the research hotspot in the always field.Traditional SERS substrate mostly uses noble metal electricity of the surface Jing Guo roughening treatment
Pole or the metal island membrane structure being made of noble metal nano colloidal solid.The common feature of these materials be surface texture it is unordered and
It is uncontrollable, it is difficult to reliable, stable, uniform SERS signal is obtained in wider dynamic range.In order to solve this problem, existing
It is used to prepare orderly noble metal nano array for nanometer etching technology.However, often there is preparation cost in these preparation means
High, many technology drawbacks such as process is many and diverse, is difficult to large area volume production, large-scale application when forbidden drug trace detection by
Limitation.Therefore, seek a kind of simple, low cost method, orderly controllable highly sensitive SERS substrate prepared to large area,
Have become critical issue urgently to be resolved at present.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing orderly gold nano cap array.
The present invention is realized by following technical solution:
A method of orderly gold nano cap array is prepared, includes the following steps: for high-purity aluminum foil to be placed in acetone and is cleaned by ultrasonic
To remove surface and oil contaminant, it is subsequently placed in ethyl alcohol and perchloric acid mixed solution that volume ratio is 6: 1 and carries out electrochemical polish, voltage
The aluminium foil that surface is in smooth mirror surface is obtained after deionized water is rinsed and is dried with nitrogen for 12-14V, time 6-8min；It will
Aluminium foil after polishing is placed in the oxalic acid solution that concentration is 0.5mol/L, and anodic oxidation 2.5- is carried out at DC voltage 34-38V
3.5h, temperature maintain 6-8 DEG C, then sample is placed in 60-70 DEG C of chromic acid and the isometric mixed solution of phosphoric acid 3-4h with
The alumina layer prepared before removal, then carries out anodic oxidation again, identical when time and condition are with first time anodic oxidation,
To obtain the PAA template of high-sequential；Sample is placed in saturation copper chloride solution and removes aluminium substrate, makes the barrier layer of PAA
It is exposed, gold is deposited on PAA barrier layer surface using electron beam evaporation deposition machine, vacuum degree is 4 × 10−3Pa, deposition speed
Rate be 0.3-0.4/s, deposition thickness be 28nm to get；Each raw material is parts by weight.
Preferably, in the method, voltage 13V.
Preferably, in the method, time 7min.
Preferably, in the method, anodic oxidation 3h is carried out at DC voltage 36V.
Preferably, in the method, temperature maintains 7 DEG C.
Preferably, in the method, sample is placed in 65 DEG C of chromic acid and the isometric mixed solution of phosphoric acid 3.5h with
The alumina layer prepared before removal.
Preferably, in the method, deposition rate is 0.35/s.
The technology of the present invention effect:
This method is easy, quick, easy to operate, and the orderly gold nano cap array of preparation increases CV molecule with strongest SERS signal
Potent fruit is expected to be applied to the trace detection of forbidden drug in aquatic products.
Specific embodiment
Essentiality content of the invention is specifically introduced below with reference to embodiment.
Embodiment 1
A method of orderly gold nano cap array is prepared, includes the following steps: for high-purity aluminum foil to be placed in acetone and is cleaned by ultrasonic
To remove surface and oil contaminant, it is subsequently placed in ethyl alcohol and perchloric acid mixed solution that volume ratio is 6: 1 and carries out electrochemical polish, voltage
The aluminium foil that surface is in smooth mirror surface is obtained after deionized water is rinsed and is dried with nitrogen for 13V, time 7min；After polishing
Aluminium foil be placed in the oxalic acid solution that concentration is 0.5mol/L, anodic oxidation 3h is carried out at DC voltage 36V, temperature maintains
7 DEG C, the aluminium oxide that sample is then placed in 3.5h in 65 DEG C of chromic acid and the isometric mixed solution of phosphoric acid to prepare before removing
Layer, then carries out anodic oxidation again, identical when time and condition are with first time anodic oxidation, to obtain high-sequential
PAA template；Sample is placed in saturation copper chloride solution and removes aluminium substrate, the barrier layer of PAA is exposed, utilizes electron beam
Gold is deposited on PAA barrier layer surface by evaporation coating machine, and vacuum degree is 4 × 10−3Pa, deposition rate are 0.35/s, deposition thickness
For 28nm to get；Each raw material is parts by weight.
Embodiment 2
A method of orderly gold nano cap array is prepared, includes the following steps: for high-purity aluminum foil to be placed in acetone and is cleaned by ultrasonic
To remove surface and oil contaminant, it is subsequently placed in ethyl alcohol and perchloric acid mixed solution that volume ratio is 6: 1 and carries out electrochemical polish, voltage
The aluminium foil that surface is in smooth mirror surface is obtained after deionized water is rinsed and is dried with nitrogen for 12V, time 6min；After polishing
Aluminium foil be placed in concentration be 0.5mol/L oxalic acid solution in, at DC voltage 34V carry out anodic oxidation 2.5h, temperature maintain
At 6 DEG C, sample is then placed in 3h in 60 DEG C of chromic acid and the isometric mixed solution of phosphoric acid to prepare before removing aluminium oxide
Layer, then carries out anodic oxidation again, identical when time and condition are with first time anodic oxidation, to obtain high-sequential
PAA template；Sample is placed in saturation copper chloride solution and removes aluminium substrate, the barrier layer of PAA is exposed, utilizes electron beam
Gold is deposited on PAA barrier layer surface by evaporation coating machine, and vacuum degree is 4 × 10−3Pa, deposition rate are 0.3/s, deposition thickness
For 28nm to get；Each raw material is parts by weight.
Embodiment 3
A method of orderly gold nano cap array is prepared, includes the following steps: for high-purity aluminum foil to be placed in acetone and is cleaned by ultrasonic
To remove surface and oil contaminant, it is subsequently placed in ethyl alcohol and perchloric acid mixed solution that volume ratio is 6: 1 and carries out electrochemical polish, voltage
The aluminium foil that surface is in smooth mirror surface is obtained after deionized water is rinsed and is dried with nitrogen for 14V, time 8min；After polishing
Aluminium foil be placed in concentration be 0.5mol/L oxalic acid solution in, at DC voltage 38V carry out anodic oxidation 3.5h, temperature maintain
At 8 DEG C, sample is then placed in 4h in 70 DEG C of chromic acid and the isometric mixed solution of phosphoric acid to prepare before removing aluminium oxide
Layer, then carries out anodic oxidation again, identical when time and condition are with first time anodic oxidation, to obtain high-sequential
PAA template；Sample is placed in saturation copper chloride solution and removes aluminium substrate, the barrier layer of PAA is exposed, utilizes electron beam
Gold is deposited on PAA barrier layer surface by evaporation coating machine, and vacuum degree is 4 × 10−3Pa, deposition rate are 0.4/s, deposition thickness
For 28nm to get；Each raw material is parts by weight.
This method is easy, quick, easy to operate, and the orderly gold nano cap array of preparation believes CV molecule with strongest SERS
Number reinforcing effect, is expected to be applied to the trace detection of forbidden drug in aquatic products.
Claims (7)
1. a kind of method for preparing orderly gold nano cap array, it is characterised in that include the following steps: high-purity aluminum foil being placed in third
Ultrasonic cleaning is subsequently placed in ethyl alcohol and perchloric acid mixed solution that volume ratio is 6: 1 to remove surface and oil contaminant and carries out electricity in ketone
Chemical polishing, voltage 12-14V, time 6-8min obtain surface in smooth after deionized water is rinsed and is dried with nitrogen
The aluminium foil of mirror surface；By the aluminium foil after polishing be placed in concentration be 0.5mol/L oxalic acid solution in, at DC voltage 34-38V into
Row anodic oxidation 2.5-3.5h, temperature maintain 6-8 DEG C, and sample is then placed in 60-70 DEG C of chromic acid and phosphoric acid mixes in equal volume
It closes 3-4h in solution and then carries out anodic oxidation, time and condition and first time again to remove the alumina layer prepared before
It is identical when anodic oxidation, to obtain the PAA template of high-sequential；Sample is placed in saturation copper chloride solution and removes aluminium base
The barrier layer of PAA is exposed in bottom, gold is deposited on PAA barrier layer surface using electron beam evaporation deposition machine, vacuum degree is
4×10−3Pa, deposition rate be 0.3-0.4/s, deposition thickness be 28nm to get；Each raw material is parts by weight.
2. according to the method described in claim 1, it is characterized by: voltage is 13V.
3. according to the method described in claim 1, it is characterized by: the time is 7min.
4. according to the method described in claim 1, it is characterized by: carrying out anodic oxidation 3h at DC voltage 36V.
5. according to the method described in claim 1, it is characterized by: temperature maintains 7 DEG C.
6. according to the method described in claim 1, it is characterized by: sample is placed in 65 DEG C of chromic acid and phosphoric acid mixes in equal volume
3.5h is in solution to remove the alumina layer prepared before.
7. according to the method described in claim 1, it is characterized by: deposition rate is 0.35/s.
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| CN201811115626.1A CN109234681A (en) | 2018-09-25 | 2018-09-25 | A method of preparing orderly gold nano cap array |
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| CN201811115626.1A CN109234681A (en) | 2018-09-25 | 2018-09-25 | A method of preparing orderly gold nano cap array |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111650081A (en) * | 2020-06-16 | 2020-09-11 | 长春黄金研究院有限公司 | Method for measuring gold quality and harmful elements in gold of pure silver gold-plated jewelry |
-
2018
- 2018-09-25 CN CN201811115626.1A patent/CN109234681A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111650081A (en) * | 2020-06-16 | 2020-09-11 | 长春黄金研究院有限公司 | Method for measuring gold quality and harmful elements in gold of pure silver gold-plated jewelry |
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