CN105203511A - Preparation method of substrate with fluorescence enhancement effect - Google Patents

Preparation method of substrate with fluorescence enhancement effect Download PDF

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Publication number
CN105203511A
CN105203511A CN201510583693.6A CN201510583693A CN105203511A CN 105203511 A CN105203511 A CN 105203511A CN 201510583693 A CN201510583693 A CN 201510583693A CN 105203511 A CN105203511 A CN 105203511A
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China
Prior art keywords
substrate
preparation
template
gold
aluminium
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CN201510583693.6A
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Chinese (zh)
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杜的洋
邱腾
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Southeast University
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Southeast University
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Priority to CN201510583693.6A priority Critical patent/CN105203511A/en
Publication of CN105203511A publication Critical patent/CN105203511A/en
Pending legal-status Critical Current

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  • Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention provides a preparation method of a substrate with a fluorescence enhancement effect. The method includes the following steps of firstly, deoxidizing aluminum oxide to obtain aluminum of a micro-nanometer structure to serve as a template of the substrate; secondly, plating the whole surface of the template of the substrate with a layer of gold in a thermal evaporation mode; thirdly, placing the aluminum template with the layer of gold attached to the surface in a vacuum tubular furnace to be subjected to thermal treatment, and obtaining the final substrate after cooling. Aluminum of the micro-nanometer structure is used as the substrate, the structure is obvious, preparation is convenient, and repeatability and stability are high; the fluoresce intensity of dyed cells on the substrate prepared through the method can be improved, and the resolution ratio can be increased.

Description

A kind of preparation method with the substrate of Fluorescence Increasing effect
Technical field
The present invention relates to a kind of preparation method with the substrate of Fluorescence Increasing effect, be directed to the substrate used in the observation of biological stain cell under fluorescent microscope and testing process especially.
Background technology
Detection technique of fluorescence, as a kind of modern spectral technique of maturation, because of advantages such as its highly sensitive and method are various, has been widely used in various analysis and characterization process.But along with people are to the further investigation of microworld, the method that tradition improves fluoroscopic examination sensitivity due to its universality poor, cannot meet all testing requirements therefore, the sensitivity improving fluoroscopic examination further has become the forward position of spectral investigation.
In numerous spectral imaging technology, cell fluorescence imaging is due to high specificity, highly sensitive, and observation is convenient, and become the means that medical diagnosis and scientific research are now indispensable, wherein, the mode of dye marker fluorescence imaging obtains to be applied the most widely.But dye marker fluorescence imaging to photo-labile, easily there is photobleaching and easily produce the shortcomings such as self-quenching to limit its further developing in biology, medical science.
Surface-enhanced fluorescence technology can catch and faint optical signalling its emissive porwer greatly being increased, and the light intensity that this greatly reduces required for fluorescence excitation, the dependence for light intensity in dye marker fluorescence imaging can be effectively reduced, and then reduce its instability for light, avoid the generation of photobleaching phenomenon.Simultaneously, surface-enhanced fluorescence technology, due to the electron transfer characteristic of its uniqueness, can well avoid the self-quenching effect of luminescent dye molecule.Surface-enhanced fluorescence also has the feature of Selective long-range DEPT, which avoid the interference of noise and background, can the detectivity of actualizing technology aspect, and resolvability, more contributes to the research of cell primary fluorescence detection.
Summary of the invention
Technical matters: for above-mentioned technology Problems existing and deficiency, the object of this invention is to provide a kind of preparation method with the substrate simple, with low cost of surface-enhanced fluorescence effect, structure, the suprabasil fluorescence intensity that staining cell can be made to prepare in the method is improved, and increases resolution.
Technical scheme: for achieving the above object, the technical scheme that a kind of preparation method with the substrate of Fluorescence Increasing effect of the present invention adopts is as follows:
1) aluminium oxide deoxidation, obtains and has the aluminium of micro nano structure as the template of substrate;
2) use the mode of thermal evaporation at whole surperficial evaporation one deck gold of the template of substrate;
3) vacuum tube furnace is put into the aluminum alloy pattern plate of one deck gold in surface and do thermal treatment, after final cooling, obtain final substrate.
The starting material aluminium of described aluminium oxide and the purity of gold are 99.99%; The aluminium oxide used is for secondary or be repeatedly oxidized.
The mode of described use thermal evaporation is golden at whole surperficial evaporation one deck of the template of substrate, or uses the mode of magnetron sputtering to substitute, and the thickness of gold is 5-15nm.
Described heat treated temperature is 350-450 DEG C.
Beneficial effect: use and have the aluminium of micro nano structure as substrate, structure is obvious, easy to prepare, repeatable and stability is high; The suprabasil fluorescence intensity that staining cell can be made to prepare in the method is improved, and increases resolution.
Use the LSPR characteristic of gold, strengthen the fluorescent characteristic of dye molecule;
Composite structure is easy to prepare, can reuse, and can stablize preservation for a long time in atmosphere.
Embodiment
A. the method for secondary oxidation is used to prepare the aluminium substrate template with structure
First be the aluminium flake (3cm*3cm, purity is 99.99%) of 0.5mm by thickness, be first placed in ultrapure water, then put into ethanol ultrasonic cleaning, remove surface and oil contaminant.Put it into again in polishing fluid and carry out polishing, remove surface oxide layer.Polishing fluid is the mixed solution of ethanol and perchloric acid, and ratio is 4:1 ~ 5:1, and is placed on Cord blood in refrigerator.
Put into customized vessel after aluminium flake after polishing being used ultrapure water cleaning and carry out oxidation processes, the method that oxidation uses is anodised mode.Wherein, aluminium flake is as anode, and the molybdenum sheet of inertia is as negative electrode, and the oxalic acid solution that the solution of use is 0.5M, the temperature of reaction is 4 DEG C, and the reaction time is 2h.
After being oxidized, the sample prepared being put into deoxidation agent and carries out deoxidation process.Wherein the consisting of of deoxidation agent, the chromic acid solution of 1.8% and the phosphoric acid solution of 6%, its volume ratio is 1:1.The reaction unit of deoxidation is placed in the water bath with thermostatic control of 75 DEG C and reacts 2h, obtain the sample after deoxidation.
The step that repeated oxidation and district are oxidized, the aluminium with micro nano structure finally obtained as the aluminium flake of the template of substrate, as the template of final substrate.
B. the mode of thermal evaporation is used to have aluminium substrate plated surface one deck gold of micro nano structure
Using the aluminium substrate with micro nano structure of acquisition as template, use the mode of thermal evaporation at body structure surface evaporation one deck gold.Wherein vacuum level requirements is for being less than 4e10 -4pa, the gold that wherein evaporation uses is High Purity Gold particle (buy from middle promise green wood, purity is 99.999%), and the temperature of evaporation is room temperature, and evaporation rate is less than thickness is 5-10nm.
C. the aluminum alloy pattern plate with gold is heat-treated, obtain final substrate
The sample substrate surface that above-mentioned steps obtains with gold is placed in vacuum tube furnace heat-treats.Heat treated mode is, 30min is warming up to 350-450 DEG C, keeps 2h at this temperature, directly opens, and is cooled to room temperature.The sample that thermal treatment obtains for needed for there is the substrate of Fluorescence Increasing effect.

Claims (4)

1. there is a preparation method for the substrate of Fluorescence Increasing effect, it is characterized in that the method comprises the following steps:
1) aluminium oxide deoxidation, obtains and has the aluminium of micro nano structure as the template of substrate;
2) use the mode of thermal evaporation at whole surperficial evaporation one deck gold of the template of substrate;
3) vacuum tube furnace is put into the aluminum alloy pattern plate of one deck gold in surface and do thermal treatment, after final cooling, obtain final substrate.
2. a kind of preparation method with the substrate of Fluorescence Increasing effect according to claim 1, is characterized in that the starting material aluminium of described aluminium oxide and the purity of gold are 99.99%; The aluminium oxide used is for secondary or be repeatedly oxidized.
3. a kind of preparation method with the substrate of Fluorescence Increasing effect according to claim 1, it is characterized in that the whole surperficial evaporation one deck gold of the mode of described use thermal evaporation in the template of substrate, or using the mode of magnetron sputtering to substitute, the thickness of gold is 5-15nm.
4. a kind of preparation method with the substrate of Fluorescence Increasing effect according to claim 1, is characterized in that described heat treated temperature is 350-450 DEG C.
CN201510583693.6A 2015-09-14 2015-09-14 Preparation method of substrate with fluorescence enhancement effect Pending CN105203511A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
CN201510583693.6A CN105203511A (en) 2015-09-14 2015-09-14 Preparation method of substrate with fluorescence enhancement effect

Publications (1)

Publication Number Publication Date
CN105203511A true CN105203511A (en) 2015-12-30

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Citations (9)

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Publication number Priority date Publication date Assignee Title
CN102001619A (en) * 2010-10-19 2011-04-06 东南大学 Substrate for fluorescence labeling cell imaging and preparation method and application thereof
WO2011133143A1 (en) * 2010-04-20 2011-10-27 Hewlett-Packard Development Company, L.P. Multi-pillar structure for molecular analysis
CN102382648A (en) * 2011-09-22 2012-03-21 天津理工大学 Method for enhancing photosynthesis spectral intensity of LED phosphor by using plasma
CN102706843A (en) * 2012-05-31 2012-10-03 东南大学 Method for preparing transparent biological substrate with spectral enhancement function
CN102774807A (en) * 2012-07-05 2012-11-14 上海大学 Method for preparing core shell type nanowire array raman scattering reinforcement substrate
CN102901715A (en) * 2012-11-07 2013-01-30 吉林大学 Fluorescence enhanced microarray biochip based on micro/nano periodic structures and method for preparing same
CN102998297A (en) * 2012-12-11 2013-03-27 东南大学 Porous microscale reaction plate for surface enhanced Raman scattering spectrum analysis
CN103194752A (en) * 2013-03-27 2013-07-10 中国科学院合肥物质科学研究院 Gold micron feather cluster modified with silver nanoparticles and preparation method and application thereof
CN103837517A (en) * 2014-03-25 2014-06-04 哈尔滨工业大学 Preparation method of metal film/zinc oxide (ZnO) nanorod array fluorescence enhancement material

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011133143A1 (en) * 2010-04-20 2011-10-27 Hewlett-Packard Development Company, L.P. Multi-pillar structure for molecular analysis
CN102001619A (en) * 2010-10-19 2011-04-06 东南大学 Substrate for fluorescence labeling cell imaging and preparation method and application thereof
CN102382648A (en) * 2011-09-22 2012-03-21 天津理工大学 Method for enhancing photosynthesis spectral intensity of LED phosphor by using plasma
CN102706843A (en) * 2012-05-31 2012-10-03 东南大学 Method for preparing transparent biological substrate with spectral enhancement function
CN102774807A (en) * 2012-07-05 2012-11-14 上海大学 Method for preparing core shell type nanowire array raman scattering reinforcement substrate
CN102901715A (en) * 2012-11-07 2013-01-30 吉林大学 Fluorescence enhanced microarray biochip based on micro/nano periodic structures and method for preparing same
CN102998297A (en) * 2012-12-11 2013-03-27 东南大学 Porous microscale reaction plate for surface enhanced Raman scattering spectrum analysis
CN103194752A (en) * 2013-03-27 2013-07-10 中国科学院合肥物质科学研究院 Gold micron feather cluster modified with silver nanoparticles and preparation method and application thereof
CN103837517A (en) * 2014-03-25 2014-06-04 哈尔滨工业大学 Preparation method of metal film/zinc oxide (ZnO) nanorod array fluorescence enhancement material

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KAMILLA MALEK ET AL.: "SERS imaging of silver coated nanostructured Al and Al2O3 substrates. The effect of nanostructure", 《JOURNAL OF RAMAN SPECTROSCOPY》 *
纪南: "利用阳极氧化铝模板制备表面增强拉曼散射活性基底", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 *
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Application publication date: 20151230