CN104316508A - Method for preparing SERS active substrate with silver nanoparticles in linear distribution - Google Patents
Method for preparing SERS active substrate with silver nanoparticles in linear distribution Download PDFInfo
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- CN104316508A CN104316508A CN201410558610.3A CN201410558610A CN104316508A CN 104316508 A CN104316508 A CN 104316508A CN 201410558610 A CN201410558610 A CN 201410558610A CN 104316508 A CN104316508 A CN 104316508A
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Abstract
The invention discloses a method for preparing an SERS active substrate with silver nanoparticles in linear distribution. The method comprises the following steps: enabling hydrofluoric acid to react with a silicon wafer, so that a Si-H bond layer covers the polished surface of the silicon wafer; reducing silver ions in silver nitrate solution through Si-H bonds so as to generate silver nanoparticles on the polished surface of the silicon wafer, so that the silver nanoparticles are linearly and orderly arranged on the surface of the silicon wafer under dual actions of the uniform electric field and flowing silver nitrate solution; and obtaining the SERS active substrate with silver nanoparticles in linear distribution. The method has the advantages of simple process flow, low cost and low time consumption; and moreover, because the silver nanoparticles in linear distribution are fixed on the polished surface of the silicon wafer, the prepared SERS active substrate with silver nanoparticles in linear distribution has high signal stability and repeatability and also has extremely high signal enhancement ability.
Description
Technical field
The present invention relates to a kind of substrate preparation method, especially relate to the preparation method that a kind of Nano silver grain is SERS (Surface-enhanced Raman Scattering, the SERS) active substrate of line style distribution.
Background technology
Nano silver grain, because of the optics of the uniqueness relevant to its size, electricity and magnetic property, receives the concern of people day by day.At present, the preparation of Nano silver grain mainly contains physical method and chemical method two class, and physical method comprises physical crushing method, vacuum condensation method and mechanical attrition method etc.; Chemical method comprises chemical reduction method, electrochemical reducing, photoreduction met hod, solution-air two phase process, microemulsion method and sol-gal process etc.Nano silver grain is as excellent catalysis material and photoelectron material, be widely used in the field such as chemical industry, optoelectronic device, as compared to the noble metal nano particles such as gold, palladium and platinum, Nano silver grain has low cost, wide local surface plasma resonance wavelength coverage and strong Surface enhanced raman spectroscopy (Surface-enhanced Raman Scattering, SERS) effect, makes it more with potential applications in the field such as optics and bio-sensing.
Raman spectrum analysis technology has fast, can't harm, sensitivity high, has been widely used in the determination and analysis of biochemical material and medicine.Raman spectrum analysis technology can combine with the Surface enhanced raman spectroscopy characteristic of noble metal nano particles, by preparing the SERS active-substrate with high enhancing ability, to realizing high detection sensitivity.At present, prepare SERS active-substrate and have following several method: the nanoparticle sol that (1) utilizes chemical synthesis process to prepare is directly as SERS active-substrate; (2) in ordered template, utilize the method plated metal nano particles such as physics, chemistry or galvanochemistry, obtain the SERS active-substrate of orderly metal nano particles array; (3) utilize parents' molecule, by electrostatic or chemical method metal nanoparticle self assembly is fixed in solid substrate (silicon chip or glass etc.) and forms SERS active-substrate.More above-mentioned three kinds of methods, first method technique is simple, and can prepare by mass, but the Raman signal of the SERS active-substrate prepared enhancing ability is relatively weak; The SERS active-substrate that second method prepares has higher Raman signal and strengthens ability, good signal stabilization and repeatability, but preparation process is by the restriction of ordered template, complex process; The SERS active-substrate that the third method prepares has good signal stabilization and repeatability, but Raman signal enhancing ability is more weak.
Summary of the invention
Technical matters to be solved by this invention is to provide the preparation method that the simple Nano silver grain of a kind of technological process is the SERS active-substrate of line style distribution, and its SERS active-substrate prepared has high Raman signal and strengthens ability, good signal stabilization and repeatability.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of Nano silver grain is the preparation method of the SERS active-substrate of line style distribution, it is characterized in that comprising the following steps:
1. the silicon chip of single-sided polishing is immersed in clean-out system completely, in clean-out system, Ultrasonic Cleaning is carried out 20 ~ 40 minutes to silicon chip, then use the silicon chip after deionized water rinsing Ultrasonic Cleaning, then drying process is carried out to the silicon chip rinsed well;
2. under condition of ice bath, be the ratio of 1:3 by volume, by mass percent concentration be 20% ~ 40% superoxol slowly to join mass percent concentration be in the concentrated sulfuric acid solution of 80% ~ 98%, carry out stirring simultaneously and superoxol and concentrated sulfuric acid solution mixed obtain oxidizing agent solution;
3. the silicon chip after 1. processing through step is immersed in the oxidizing agent solution 2. prepared by step completely, and make silicon chip in oxidizing agent solution, react 0.5 ~ 1 hour to remove the organism on silicon chip, take out the silicon chip of organics removal afterwards, again with the silicon chip several of deionized water rinsing organics removal, finally drying process is carried out to the silicon chip rinsed well;
4. the silicon chip after 3. processing through step being immersed mass percent concentration is completely in the hydrofluoric acid solution of 5% ~ 25%, and makes silicon chip react 0.5 ~ 1 hour in a solution of hydrofluoric acid to form Si-H key on the polished surface of silicon chip;
5. be that the reaction vessel of the liquor argenti nitratis ophthalmicus of 0.1% ~ 2% is placed in the uniform electric field that electric field intensity is 1kV/m ~ 20kV/m by being equipped with mass percent concentration, then utilize constant flow pump that liquor argenti nitratis ophthalmicus is flowed along the direction of an electric field of uniform electric field, and flow is 50ml/min ~ 500ml/min, again the silicon chip after 4. processing through step is immersed in the liquor argenti nitratis ophthalmicus of flowing completely, Nano silver grain is generated to make the Si-H key reduction silver ion on the polished surface of silicon chip, and Nano silver grain grows along the direction of an electric field of uniform electric field, react to take out after 1 ~ 3 minute and be formed with the silicon chip that Nano silver grain is line style distribution, finally to be formed Nano silver grain be line style distribution silicon chip carry out drying process, namely the SERS active-substrate that Nano silver grain is line style distribution is prepared.At this, the silicon chip being coated with Si-H key is immersed in liquor argenti nitratis ophthalmicus, Si-H key can reduce silver ion and grow on the polished surface of silicon chip and obtain Nano silver grain, and the at the uniform velocity flowing of added uniform electric field and reaction solution in reduction process, the growth pattern of Nano silver grain can be affected.
Described step 1. in clean-out system be toluene or ethanol or acetone; At this, clean-out system also can select other organic reagent.
Described step 1. with described step 3. in deionization resistivity of water be 18.2M Ω cm.
Described step 5. in uniform electric field produced by two pieces of parallel sheet metals, and the electric field in region residing for silicon chip is uniform electric field to require the size on the surface of sheet metal to ensure.
Compared with prior art, the invention has the advantages that: the inventive method adopts chemical reduction method to generate Nano silver grain on the polished surface of silicon chip, then under the double influence of the mobilization power of uniform electric field and liquor argenti nitratis ophthalmicus, Nano silver grain on the polished surface of silicon chip is grown along the direction of an electric field of uniform electric field, obtain the SERS active-substrate that Nano silver grain is line style distribution, technological process is simple, cost is low, consuming time few, and because Nano silver grain is that line style distribution is fixed on the polished surface of silicon chip, therefore the Nano silver grain prepared be line style distribution SERS active-substrate there is good signal stabilization and repeatability, there is fabulous signal simultaneously and strengthen ability.
Accompanying drawing explanation
Atomic force microscope (AFM) image of Fig. 1 to be Nano silver grain that method that embodiment one provides prepares be SERS active-substrate of line style distribution;
The SERS active-substrate of Fig. 2 to be Nano silver grain that method that embodiment one provides prepares be line style distribution carries out Raman signal detection to Raman labels molecule 4 mercaptobenzoic acid (4MBA), the Raman spectrogram obtained;
Atomic force microscope (AFM) image of Fig. 3 to be Nano silver grain that method that embodiment two provides prepares be SERS active-substrate of line style distribution;
The SERS active-substrate of Fig. 4 to be Nano silver grain that method that embodiment two provides prepares be line style distribution carries out Raman signal detection to Raman labels molecule 4 mercaptobenzoic acid (4MBA), the Raman spectrogram obtained;
Atomic force microscope (AFM) image of Fig. 5 to be Nano silver grain that method that embodiment three provides prepares be SERS active-substrate of line style distribution;
The SERS active-substrate of Fig. 6 to be Nano silver grain that method that embodiment three provides prepares be line style distribution carries out Raman signal detection to Raman labels molecule 4 mercaptobenzoic acid (4MBA), the Raman spectrogram obtained;
Atomic force microscope (AFM) image of Fig. 7 to be Nano silver grain that method that embodiment four provides prepares be SERS active-substrate of line style distribution;
The SERS active-substrate of Fig. 8 to be Nano silver grain that method that embodiment four provides prepares be line style distribution carries out Raman signal detection to Raman labels molecule 4 mercaptobenzoic acid (4MBA), the Raman spectrogram obtained.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment one:
A kind of Nano silver grain that the present embodiment proposes is the preparation method of the SERS active-substrate of line style distribution, and it comprises the following steps:
1. the silicon chip that one piece of length of side is the foursquare single-sided polishing of 5mm is chosen, the silicon chip of single-sided polishing is immersed in clean-out system completely, in clean-out system, Ultrasonic Cleaning is carried out 30 minutes to silicon chip, then use the silicon chip after deionized water rinsing Ultrasonic Cleaning, then drying process is carried out to the silicon chip rinsed well.
At this, the silicon chip of single-sided polishing also can select the silicon chip of other shape and size; Clean-out system is toluene or the organic reagent such as ethanol or acetone; Deionized water employing resistivity is the deionized water of 18.2M Ω cm; Dry process adopts the Drying Treatment Technology of existing maturation.
When reality is implemented, the time of silicon chip being carried out to Ultrasonic Cleaning is not strict with, generally 20 ~ 40 minutes capable of washing, ensures Wafer Cleaning totally.
2. under condition of ice bath, be the ratio of 1:3 by volume, by mass percent concentration be 30% superoxol slowly to join mass percent concentration be in the concentrated sulfuric acid solution of 98%, carry out stirring simultaneously and superoxol and concentrated sulfuric acid solution mixed obtain oxidizing agent solution.The mass percent concentration getting 15ml is in the concentrated sulfuric acid solution implantation glass beaker of 98%, then glass beaker is placed in the container of the potpourri that ice cube and water are housed, the mass percent concentration getting 5ml is again the superoxol of 30%, slowly be added drop-wise in concentrated sulfuric acid solution, stir while dripping, leave standstill 10 minutes after stirring, namely prepare oxidizing agent solution.
In this step, the concentration of the oxidizing agent solution of preparation is determined by the concentration of the dense and concentrated sulfuric acid solution of superoxol used in preparation process, shorter with the time required for the attachment on the oxidizing agent solution of high concentration thorough cleaning silicon chip surface; And it is longer with the time required for the attachment on the oxidizing agent solution of low concentration thorough cleaning silicon chip surface.
3. the silicon chip after 1. processing through step is immersed in the oxidizing agent solution 2. prepared by step completely, and make silicon chip in oxidizing agent solution, react 0.8 hour to remove the organism on silicon chip, take out the silicon chip of organics removal afterwards, again with the silicon chip several of deionized water rinsing organics removal, finally drying process is carried out to the silicon chip rinsed well.
When reality is implemented, the reaction time of silicon chip in oxidizing agent solution is generally 0.5 ~ 1 hour, only requires the organism removed completely on silicon chip.
At this, deionized water employing resistivity is the deionized water of 18.2M Ω cm; Dry process adopts the Drying Treatment Technology of existing maturation.
4. the silicon chip after 3. processing through step being immersed mass percent concentration is completely in the hydrofluoric acid solution of 5%, and makes silicon chip react 0.5 hour in a solution of hydrofluoric acid to form Si-H key on the polished surface of silicon chip.
5. be that the reaction vessel of the liquor argenti nitratis ophthalmicus of 0.1% is placed in the uniform electric field that electric field strength is 1kV/m by being equipped with mass percent concentration, then utilize existing constant flow pump that liquor argenti nitratis ophthalmicus is flowed along the direction of an electric field of uniform electric field, and flow is 50ml/min, again the silicon chip after 4. processing through step is immersed in the liquor argenti nitratis ophthalmicus of flowing completely, Nano silver grain is generated to make the Si-H key reduction silver ion on the polished surface of silicon chip, and Nano silver grain grows along the direction of an electric field of uniform electric field, react to take out after 1 minute and be formed with the silicon chip that Nano silver grain is line style distribution, finally to be formed Nano silver grain be line style distribution silicon chip carry out drying process, namely the SERS active-substrate that Nano silver grain is line style distribution is prepared.
Fig. 1 gives atomic force microscope (AFM) image that Nano silver grain that said method prepares is the SERS active-substrate of line style distribution.As can be seen from Figure 1, the particle size of the Nano silver grain in this SERS active-substrate is between 20 ~ 200nm; Under the double influence of the mobilization power of additional uniform electric field and liquor argenti nitratis ophthalmicus, Nano silver grain on silicon chip is line bunch formula distribution along direction of an electric field, and on parallel electric field direction, gap between Nano silver grain is less, and on vertical electric field direction, the gap between Nano silver grain is larger.
It is that the SERS active-substrate of line style distribution carries out Raman signal detection to Raman labels molecule 4 mercaptobenzoic acid (4MBA), the Raman spectrogram obtained that Fig. 2 gives Nano silver grain that said method prepares.During detection, the concentration of 4MBA solution used is 3.6 × 10
-8mol/L, the power of laser used is 49.95mW, and integral time is 10s.As can be seen from Figure 2, this SERS active-substrate has good SERS signal enhancement effect, and it is at 1078cm
-1the Raman signal intensity at place reaches 35000.
Embodiment two:
A kind of Nano silver grain that the present embodiment proposes be that the process of preparation method of the SERS active-substrate that line style distributes is substantially identical with the process of the preparation method that embodiment one provides, difference is that the mass percent concentration of the hydrofluoric acid solution that the present embodiment adopts is 10%, the silicon chip reaction time be immersed in hydrofluoric acid solution is 0.7 hour, additional uniform electric field intensity is 4kV/m, the mass percent concentration of liquor argenti nitratis ophthalmicus is 1%, the flow of liquor argenti nitratis ophthalmicus is 300ml/min, and the silicon chip reaction time be immersed in liquor argenti nitratis ophthalmicus is 1.5 minutes.Namely the step of the preparation method of the present embodiment is 1. 3. 1. 3. identical to step with the step of the preparation method of embodiment one to step, 4. the step of the preparation method of the present embodiment with step process is 5.: 4. the silicon chip after 3. processing through step being immersed mass percent concentration is completely in the hydrofluoric acid solution of 10%, and makes silicon chip react 0.8 hour in a solution of hydrofluoric acid to form Si-H key on the polished surface of silicon chip, 5. be that the reaction vessel of the liquor argenti nitratis ophthalmicus of 1% is placed in the uniform electric field that electric field strength is 4kV/m by being equipped with mass percent concentration, then liquor argenti nitratis ophthalmicus is made to flow along the direction of an electric field of uniform electric field, and flow is 300ml/min, again the silicon chip after 4. processing through step is immersed in the liquor argenti nitratis ophthalmicus of flowing completely, Nano silver grain is generated to make the Si-H key reduction silver ion on the polished surface of silicon chip, and Nano silver grain grows along the direction of an electric field of uniform electric field, react to take out after 1.5 minutes be formed Nano silver grain be line style distribution silicon chip, finally to be formed Nano silver grain be line style distribution silicon chip carry out drying process, namely the SERS active-substrate that Nano silver grain is line style distribution is prepared.
Fig. 3 gives atomic force microscope (AFM) image that Nano silver grain that said method prepares is the SERS active-substrate of line style distribution.As can be seen from Figure 3, the particle size of the Nano silver grain in this SERS active-substrate is between 200 ~ 600nm; Under the double influence of the mobilization power of additional uniform electric field and liquor argenti nitratis ophthalmicus, Nano silver grain on silicon chip is along direction of an electric field bunch formula distribution in closely regular line, and on parallel electric field direction, gap between Nano silver grain is less, and on vertical electric field direction, the gap between Nano silver grain is larger.
It is that the SERS active-substrate of line style distribution carries out Raman signal detection to Raman labels molecule 4 mercaptobenzoic acid (4MBA), the Raman spectrogram obtained that Fig. 4 gives Nano silver grain that said method prepares.During detection, the concentration of 4MBA solution used is 3.6 × 10
-8mol/L, the power of laser used is 49.95mW, and integral time is 10s.As can be seen from Figure 4, this SERS active-substrate has good SERS signal enhancement effect, and it is at 1078cm
-1the Raman signal intensity at place reaches 48000.
The Nano silver grain prepared compared to embodiment one is the SERS active-substrate of line style distribution, and the Nano silver grain that the present embodiment prepares be that the SERS active-substrate that distributes of line style has stronger SERS signal enhancement effect.
Embodiment three:
A kind of Nano silver grain that the present embodiment proposes be that the process of preparation method of the SERS active-substrate that line style distributes is substantially identical with the process of the preparation method that embodiment one provides, difference is that the mass percent concentration of the hydrofluoric acid solution that the present embodiment adopts is 20%, the silicon chip reaction time be immersed in hydrofluoric acid solution is 0.8 hour, additional uniform electric field intensity is 10kV/m, the mass percent concentration of liquor argenti nitratis ophthalmicus is 1.5%, the flow of liquor argenti nitratis ophthalmicus is 400ml/min, and the silicon chip reaction time be immersed in liquor argenti nitratis ophthalmicus is 2 minutes.Namely the step of the preparation method of the present embodiment is 1. 3. 1. 3. identical to step with the step of the preparation method of embodiment one to step, 4. the step of the preparation method of the present embodiment with step process is 5.: 4. the silicon chip after 3. processing through step being immersed mass percent concentration is completely in the hydrofluoric acid solution of 20%, and makes silicon chip react 0.8 hour in a solution of hydrofluoric acid to form Si-H key on the polished surface of silicon chip, 5. be that the reaction vessel of the liquor argenti nitratis ophthalmicus of 1.5% is placed in the uniform electric field that electric field strength is 10kV/m by being equipped with mass percent concentration, then liquor argenti nitratis ophthalmicus is made to flow along the direction of an electric field of uniform electric field, and flow is 400ml/min, again the silicon chip after 4. processing through step is immersed in the liquor argenti nitratis ophthalmicus of flowing completely, Nano silver grain is generated to make the Si-H key reduction silver ion on the polished surface of silicon chip, and Nano silver grain grows along the direction of an electric field of uniform electric field, react to take out after 2 minutes be formed Nano silver grain be line style distribution silicon chip, finally to be formed Nano silver grain be line style distribution silicon chip carry out drying process, namely the SERS active-substrate that Nano silver grain is line style distribution is prepared.
Fig. 5 gives atomic force microscope (AFM) image that Nano silver grain that said method prepares is the SERS active-substrate of line style distribution.As can be seen from Figure 5, the particle size of the Nano silver grain in this SERS active-substrate is between 30 ~ 90nm; Under the double influence of the mobilization power of additional uniform electric field and liquor argenti nitratis ophthalmicus, Nano silver grain on silicon chip is along direction of an electric field bunch formula distribution in closely regular line, and on parallel electric field direction, gap between Nano silver grain is less, and on vertical electric field direction, the gap between Nano silver grain is larger.
It is that the SERS active-substrate of line style distribution carries out Raman signal detection to Raman labels molecule 4 mercaptobenzoic acid (4MBA), the Raman spectrogram obtained that Fig. 6 gives Nano silver grain that said method prepares.During detection, the concentration of 4MBA solution used is 3.6 × 10
-8mol/L, the power of laser used is 49.95mW, and integral time is 10s.As can be seen from Figure 6, this SERS active-substrate has good SERS signal enhancement effect, and it is at 1078cm
-1the Raman signal intensity at place reaches 50000.
The Nano silver grain prepared compared to embodiment one and embodiment two be the SERS active-substrate that line style distributes, and the Nano silver grain that the present embodiment prepares is that the SERS active-substrate that distributes of line style has stronger SERS signal enhancement effect.
Embodiment four:
A kind of Nano silver grain that the present embodiment proposes be that the process of preparation method of the SERS active-substrate that line style distributes is substantially identical with the process of the preparation method that embodiment one provides, difference is that the mass percent concentration of the hydrofluoric acid solution that the present embodiment adopts is 25%, the silicon chip reaction time be immersed in hydrofluoric acid solution is 1 hour, additional uniform electric field intensity is 20kV/m, the mass percent concentration of liquor argenti nitratis ophthalmicus is 2%, the flow of liquor argenti nitratis ophthalmicus is 500ml/min, and the silicon chip reaction time be immersed in liquor argenti nitratis ophthalmicus is 3 minutes.Namely the step of the preparation method of the present embodiment is 1. 3. 1. 3. identical to step with the step of the preparation method of embodiment one to step, 4. the step of the preparation method of the present embodiment with step process is 5.: 4. the silicon chip after 3. processing through step being immersed mass percent concentration is completely in the hydrofluoric acid solution of 25%, and makes silicon chip react 0.8 hour in a solution of hydrofluoric acid to form Si-H key on the polished surface of silicon chip, 5. be that the reaction vessel of the liquor argenti nitratis ophthalmicus of 2% is placed in the uniform electric field that electric field strength is 20kV/m by being equipped with mass percent concentration, then liquor argenti nitratis ophthalmicus is made to flow along the direction of an electric field of uniform electric field, and flow is 500ml/min, again the silicon chip after 4. processing through step is immersed in the liquor argenti nitratis ophthalmicus of flowing completely, Nano silver grain is generated to make the Si-H key reduction silver ion on the polished surface of silicon chip, and Nano silver grain grows along the direction of an electric field of uniform electric field, react to take out after 3 minutes be formed Nano silver grain be line style distribution silicon chip, finally to be formed Nano silver grain be line style distribution silicon chip carry out drying process, namely the SERS active-substrate that Nano silver grain is line style distribution is prepared.
Fig. 7 gives atomic force microscope (AFM) image that Nano silver grain that said method prepares is the SERS active-substrate of line style distribution.As can be seen from Figure 7, the particle size of the Nano silver grain in this SERS active-substrate is about 100nm, be that the SERS active-substrate that distributes of line style is compared with embodiment one, embodiment two and the preparation-obtained Nano silver grain of embodiment three, the Nano silver grain that the present embodiment prepares is that the domain size distribution of Nano silver grain in the SERS active-substrate of line style distribution is more even, and presents the line bunch arrangement of more closely rule.
It is that the SERS active-substrate of line style distribution carries out Raman signal detection to Raman labels molecule 4 mercaptobenzoic acid (4MBA), the Raman spectrogram obtained that Fig. 8 gives Nano silver grain that said method prepares.During detection, the concentration of 4MBA solution used is 3.6 × 10
-8mol/L, the power of laser used is 49.95mW, and integral time is 10s.As can be seen from Figure 8, this SERS active-substrate has good SERS signal enhancement effect, and it is at 1078cm
-1the Raman signal intensity at place reaches 54500.
The Nano silver grain prepared with embodiment three compared to embodiment one, embodiment two be the SERS active-substrate that line style distributes, and the Nano silver grain that the present embodiment prepares is that the SERS active-substrate that distributes of line style has the strongest SERS signal enhancement effect.
Claims (4)
1. Nano silver grain is a preparation method for the SERS active-substrate of line style distribution, it is characterized in that comprising the following steps:
1. the silicon chip of single-sided polishing is immersed in clean-out system completely, in clean-out system, Ultrasonic Cleaning is carried out 20 ~ 40 minutes to silicon chip, then use the silicon chip after deionized water rinsing Ultrasonic Cleaning, then drying process is carried out to the silicon chip rinsed well;
2. under condition of ice bath, be the ratio of 1:3 by volume, by mass percent concentration be 20% ~ 40% superoxol slowly to join mass percent concentration be in the concentrated sulfuric acid solution of 80% ~ 98%, carry out stirring simultaneously and superoxol and concentrated sulfuric acid solution mixed obtain oxidizing agent solution;
3. the silicon chip after 1. processing through step is immersed in the oxidizing agent solution 2. prepared by step completely, and make silicon chip in oxidizing agent solution, react 0.5 ~ 1 hour to remove the organism on silicon chip, take out the silicon chip of organics removal afterwards, again with the silicon chip several of deionized water rinsing organics removal, finally drying process is carried out to the silicon chip rinsed well;
4. the silicon chip after 3. processing through step being immersed mass percent concentration is completely in the hydrofluoric acid solution of 5% ~ 25%, and makes silicon chip react 0.5 ~ 1 hour in a solution of hydrofluoric acid to form Si-H key on the polished surface of silicon chip;
5. be that the reaction vessel of the liquor argenti nitratis ophthalmicus of 0.1% ~ 2% is placed in the uniform electric field that electric field intensity is 1kV/m ~ 20kV/m by being equipped with mass percent concentration, then utilize constant flow pump that liquor argenti nitratis ophthalmicus is flowed along the direction of an electric field of uniform electric field, and flow is 50ml/min ~ 500ml/min, again the silicon chip after 4. processing through step is immersed in the liquor argenti nitratis ophthalmicus of flowing completely, Nano silver grain is generated to make the Si-H key reduction silver ion on the polished surface of silicon chip, and Nano silver grain grows along the direction of an electric field of uniform electric field, react to take out after 1 ~ 3 minute and be formed with the silicon chip that Nano silver grain is line style distribution, finally to be formed Nano silver grain be line style distribution silicon chip carry out drying process, namely the SERS active-substrate that Nano silver grain is line style distribution is prepared.
2. a kind of Nano silver grain according to claim 1 is the preparation method of SERS active-substrate of line style distribution, and the clean-out system that it is characterized in that during described step is 1. toluene or ethanol or acetone.
3. a kind of Nano silver grain according to claim 1 and 2 is the preparation method of SERS active-substrate of line style distribution, it is characterized in that described step 1. with described step 3. in deionization resistivity of water be 18.2M Ω cm.
4. a kind of Nano silver grain according to claim 3 is the preparation method of SERS active-substrate of line style distribution, it is characterized in that uniform electric field during described step is 5. produced by two pieces of parallel sheet metals.
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| CN106513703A (en) * | 2016-11-22 | 2017-03-22 | 宁波工程学院 | Preparation method of chitosan Ag nano-composite film |
| CN112461811A (en) * | 2020-11-30 | 2021-03-09 | 西北民族大学 | Preparation method of flexible SERS substrate, prepared substrate and application of substrate |
| CN114018897A (en) * | 2021-10-21 | 2022-02-08 | 云南省产品质量监督检验研究院 | Preparation method of silicon-based SERS substrate based on double-layer silver nanostructure |
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- 2014-10-20 CN CN201410558610.3A patent/CN104316508A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105606587A (en) * | 2015-12-31 | 2016-05-25 | 宁波大学 | Enrofloxacin detection method based on silver nanoparticles and carborundum paper SERS substrate |
| CN105606587B (en) * | 2015-12-31 | 2018-09-28 | 宁波大学 | Enrofloxacin detection method based on nano-Ag particles Yu carborundum paper SERS substrates |
| CN106513703A (en) * | 2016-11-22 | 2017-03-22 | 宁波工程学院 | Preparation method of chitosan Ag nano-composite film |
| CN106513703B (en) * | 2016-11-22 | 2018-05-15 | 宁波工程学院 | A kind of preparation method of chitosan Ag nano composite membranes |
| CN112461811A (en) * | 2020-11-30 | 2021-03-09 | 西北民族大学 | Preparation method of flexible SERS substrate, prepared substrate and application of substrate |
| CN112461811B (en) * | 2020-11-30 | 2023-09-26 | 西北民族大学 | Preparation method of flexible SERS substrate, prepared substrate and application of prepared substrate |
| CN114018897A (en) * | 2021-10-21 | 2022-02-08 | 云南省产品质量监督检验研究院 | Preparation method of silicon-based SERS substrate based on double-layer silver nanostructure |
| CN114018897B (en) * | 2021-10-21 | 2023-04-07 | 云南省产品质量监督检验研究院 | Preparation method of silicon-based SERS substrate based on double-layer silver nanostructure |
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