CN108526487A - A kind of preparation method of macro-size closs packing gold nano grain monofilm - Google Patents
A kind of preparation method of macro-size closs packing gold nano grain monofilm Download PDFInfo
- Publication number
- CN108526487A CN108526487A CN201810590635.XA CN201810590635A CN108526487A CN 108526487 A CN108526487 A CN 108526487A CN 201810590635 A CN201810590635 A CN 201810590635A CN 108526487 A CN108526487 A CN 108526487A
- Authority
- CN
- China
- Prior art keywords
- gold nano
- size
- macro
- nanometers
- monofilm
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- 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
Abstract
Amine is configured to the oily solution containing amine that molar concentration is 0.0001 0.1 mol/Ls by a kind of preparation method of the closs packing gold nano grain monofilm of macro-size using oil-based solvent first；Then it uses 16 nanometers of gold nano grains as seed, seed mediated growth method is used in combination to prepare the gold nano particle colloidal sols of 30 150 nanometers of size range；It again will be by gold nano particle colloidal sols and oily solution containing amine with 5:13 volume ratio is thoroughly mixed, and is stood, and waits for upper oil phase volatilization completely to get to macro-size auri self-assembled monolayer solid matter nanometer film；Finally using soda acid, treated that sheet glass completely pulls film out, dry under vacuum or nitrogen atmosphere after rinsing surface with ethyl alcohol.The present invention is easy to operate, it can obtain the closs packing gold nano grain monofilm that can be used as Raman enhancing substrate of single layer, high quality, solid matter, macro-size, and there is uniform Surface enhanced Raman scattering performance, to realize the quantitative detection in their Raman enhancing fields.
Description
Technical field
The present invention relates to it is a kind of be used to prepare can be used as Raman enhance substrate macro-size closs packing gold nano grain list
The method of tunic belongs to noble metal nano particles self-assembling technique field.
Background technology
Surface enhanced Raman scattering is a kind of optical tooling with fingerprint specific detection, can be quick, sensitive
Trace detection biochemical molecule has many applications in medicine, biology, chemistry, optics etc..Therefore, substrate is steady
Qualitative, detection sensitivity and reproducibility are most important.Currently, people enhance Surface enhanced Raman scattering by multiple means
Stability and sensitivity, but the reproducibility of its detection is still a great problem.
The construction of substrate is to promote Surface enhanced Raman scattering detection quality critical：The material of base material, " hot spot " and
Arrangement determines its stability, sensitivity and reproducibility.Gold nano grain based on its excellent surface plasma resonance effect,
The foreground of being widely applied is illustrated in Surface enhanced Raman scattering test, there is very high detection sensitivity.Moreover, working as nanometer
Grain between gap very little (being defined as " hot spot ") when, near-field coupling will produce strong Electromagnetic enhancement, to detect it is sensitive
Also tool improves degree；If the nano particle closed on will present rule by certain periodic arrangement, Electromagnetic enhancement
Rule, directive distribution, this provides possibility for the reproducibility of Surface Enhanced Raman Scattering Spectrum and quantitative analysis.In addition,
Gold nano grain has excellent chemical stability, corrosion resistance and oxidation resistent susceptibility.Therefore the closs packing of macro-size is prepared
Gold nano grain monofilm makes it have both the intrinsic surface plasma resonance effect and chemical stability of gold nano grain, and
Regular, directive Electromagnetic enhancement is generated when being excited, and the sensitivity, steady of Surface enhanced Raman scattering test can be improved
Qualitative and reproducibility.
In the past more than ten years, the preparation about noble metal nano film has done a large amount of research, including mould there are many people
Plate substrate auxiliary law, solwution method, interface method, external force auxiliary law etc..Wherein, interface method has and does not need compared to other methods
By other substrates as template, without advantages such as external force, membrane structures easily transfer.End up to the present, by simple real
Test condition and step and closs packing gold nano grain monofilm that a step prepares macro-size is still a great problem.
Currently, the closs packing gold nano grain monofilm that can prepare macro-size is mainly to utilize the gold prepared in oil phase
Nano particle.But due to the limitation of oil phase preparation method, gold particle size can only be confined to 20 nanometers or less.Meanwhile greatly
The use for measuring organic ligand, can also limit test molecule and be adsorbed onto gold particle surface, to influence its Raman-enhancing energy.When
Before, various sizes of water-soluble gold rice grain can be easy to prepare.Therefore, with these various sizes of water-soluble gold particles
The closs packing gold nano grain monofilm for preparing macro-size expands gold particle answering in Raman enhancing field by great
With.
Currently, in the various methods of closs packing gold nano grain monofilm that interface prepares macro-size, to prevent group
The reunion for the water-soluble gold rice grain that electrostatic force is stablized during dress, often as protective agent or is made using macromolecular polymer
Nanometer film is obtained with multistep processes；Obtained film is not uniform single layer structure, has overlapping, gap；And individual particle size compared with
It is small.Prepared gold nano grain monofilm does not have uniform Raman signal, to limit in their Raman enhancing fields
Quantitative detection.In addition, the large-size for 30-150 nanometers does not have good self-assembling method.
Therefore, more Size Distributions, macro-size closs packing gold nano grain monofilm is prepared by simple one-step method
It is a no small challenge.The solution of these problems can unquestionably widen traditional gold nano grain and be examined in biomedicine significantly
The application of survey, sensor and surface Raman enhancement etc.；While ensuring stability and sensitivity, the solution of sex chromosome mosaicism is reappeared
Certainly (uniform Raman signal is presented everywhere) undoubtedly makes Raman enhanced spectrum technical research into the rank of a new quantitative detection
Section.
Invention content
The present invention is for the existing macro-size closs packing gold nano grain monofilm used as Raman enhancing substrate
It is insufficient existing for technology of preparing, a kind of system easy to operate, efficiently macro-size closs packing gold nano grain monofilm is provided
Preparation Method.This method is that the water-soluble gold rice grain for the various sizes that will be prepared is mixed with organic solvent, by organic
Amine organic molecule (octadecylamine, octadecenyl amine, the quaternary ammonium salt of addition low concentration in solvent (toluene, hexane, amylalcohol, enanthol etc.)
Deng), under its auxiliary, gold nano grain can be transferred to oil-water interfaces from water phase and be self-assembled into closely packed monofilm, institute
The macro-size of preparation, closely packed gold nano grain monofilm can have uniform Raman to enhance signal, to realize them
Quantitative detection in Raman enhancing field.
The preparation method of the macro-size closs packing gold nano grain monofilm of the present invention, includes the following steps：
(1) 16 nanometers of gold nano particle colloidal sols are prepared, and prepare 30-150 nanometers of size range using it as seed
Gold nano particle colloidal sols；
(2) using oil-based solvent by amine be configured to molar concentration be 0.0001-0.1 mol/Ls oiliness containing amine it is molten
Liquid；
(3) gold nano particle colloidal sols are pressed with oily solution containing amine with 5:The volume ratio of 1-3 is thoroughly mixed；
(4) it stands, waits for upper oil phase volatilization completely to get to the closs packing gold nano grain monofilm of macro-size；
(5) soda acid treated substrate (sheet glass, silicon chip or flexible substrates) is used, film is completely pulled out, with anhydrous second
It is dry under vacuum or nitrogen atmosphere after alcohol rinses surface.
The preparation process of 16 nanometers of gold nano particle colloidal sols is as described below in the step (1)：
1. sodium citrate and gold chloride are configured to the sodium citrate that mass percent concentration is 1% respectively using ultra-pure water
The chlorauric acid solution that solution and mass percent concentration are 1%；
2. by chlorauric acid solution and ultra-pure water 1:Chlorauric acid solution is added in boiling water by 96 volume ratio；
3. by sodium citrate solution and chlorauric acid solution 3:2. 1 volume ratio contains sodium citrate solution addition step
In the boiling water of gold chloride, become boiling mixed liquor；
4. keeping boiling, 1 hour postcooling is heated to reflux to room temperature, that is, is obtained water-soluble mono and disperseed spherical 16 nanometers
Gold nano particle colloidal sols.
The following institute of preparation process for the gold nano particle colloidal sols for preparing 30-150 nanometers of size range in the step (1)
It states：
1. trishydroxymethylaminomethane is configured to the trihydroxy methyl ammonia that molar concentration is 0.1 mol/L using ultra-pure water
Methylmethane solution；Gold chloride is configured to the chlorauric acid solution that mass percent concentration is 1% using ultra-pure water；
2. pressing tris solution, chlorauric acid solution, 16 nanometers of gold nano particle colloidal sols and ultra-pure water 4:
1:20-0.16:The volume ratio of 75-94.84, by tris solution, chlorauric acid solution, 16 nanometers of gold nano
Grain colloidal sol is added sequentially in boiling water；
3. keeping boiling, 1 hour postcooling is heated to reflux to room temperature, that is, is obtained the spherical 30-150 of water-soluble mono dispersion and received
The gold nano particle colloidal sols of rice.
The oil-based solvent is toluene, hexane, amylalcohol or enanthol.
The amine is octadecylamine, octadecenyl amine or quaternary ammonium salt.
The detailed process of the step (5) is：
Soda acid processing is carried out to substrate (sheet glass, silicon chip or flexible substrates), using soda acid treated substrate from beaker
Go deep into beaker at interior no film, and beaker is tilted into close nanometer film behind 45 degree angles；After nanometer film and flexible substrates have contact,
Slowly lifting substrate, until film is completely pulled out；Then the substrate surface for being loaded with gold nano film, juxtaposition are rinsed using absolute ethyl alcohol
It is dry under vacuum or nitrogen atmosphere.
Described refers to impregnating base using new configuration chloroazotic acid and saturation sodium hydroxide solution respectively to substrate progress soda acid processing
Bottom (sheet glass, silicon chip or flexible substrates), time 0.8-1.2 hour.
The gold nano grain that the present invention prepares 16 nanometers using classical approach is used in combination seed mediated growth method to prepare 30- as seed
150 nanometers of water solubility, monodisperse, spherical gold nano grain；Then using be dissolved in specific organic solvent (toluene, hexane,
Amylalcohol, enanthol etc.) low concentration amine (octadecylamine, octadecenyl amine, quaternary ammonium salt etc.) simply mixed with gold nano colloidal sol, be quiet
It sets, you can obtain the closs packing gold nano grain monofilm of macro-size.Compared to more other self-assembling methods, this method operation
Simply, the single layer that other existing methods are unable to get, the closs packing gold nano of high quality, solid matter, macro-size can be obtained
Grain monofilm.
Description of the drawings
Fig. 1 is that the transmission electron microscope of the closs packing gold nano grain monofilm for the macro-size that the present invention synthesizes shines
Piece.
Fig. 2 is that three of the closs packing gold nano grain monofilm for the same macro-size that the present invention synthesizes are random different
Constituency Surface Enhanced Raman Scattering Spectrum (a-c).
Specific implementation mode
Prepare gold nano particle colloidal sols using seed mediated growth method in the present invention, the seed mediated growth method by Zhang Peina, Li Yijing,
Wang great Yang and Xia Haibing was published in 2016 on Part.Part.Syst.Charact. periodicals, specifically High-Yield
Production of Uniform Gold Nanoparticles with Sizes from 31to 577nm via One-
Pot Seeded Growth and Size-Dependent SERS Property are (with high yield by a step seed mediated growth method
Prepare the size-dependent research for the uniform gold nano grain and its Surface enhanced Raman spectroscopy that grain size is 31~577 nanometers)
.Part.Part.Syst.Charact.2016,33,924–932。
The present invention prepares the gold nano particle colloidal sols of high yield, sizes with reference to the seed mediated growth method in above-mentioned document
Details are provided below：
(1) glassware used (100 milliliters of twoport flasks and 25 milliliters of beaker) is put into the chloroazotic acid newly configured and is soaked
Bubble was cleaned with sodium nitrate saturated solution and ultra-pure water, is dried for standby after 2 hours.25 milliliters of beaker need to reuse saturation hydrogen-oxygen
Change sodium solution to impregnate 12 hours or more, is cleaned, be dried for standby with sodium nitrate saturated solution and ultra-pure water；
(2) use ultra-pure water by sodium citrate (reducing agent, stabilizer), trishydroxymethylaminomethane (reducing agent, stabilization
Agent) and gold chloride (soluble precursor) be configured to respectively mass percent concentration be 1% sodium citrate solution, molar concentration
The chlorauric acid solution that tris solution and mass percent concentration for 0.1 mol/L are 1%；
(3) chlorauric acid solution and ultra-pure water 1 are pressed:Chlorauric acid solution is added in boiling water by 96 volume ratio；
(4) sodium citrate solution and chlorauric acid solution 3 are pressed:Sodium citrate solution is added step (2) and contained by 1 volume ratio
Have in the boiling water of gold chloride, becomes boiling mixed liquor；
(5) boiling is kept, 1 hour postcooling is heated to reflux to room temperature, that is, obtains spherical 16 nanometers of water-soluble mono dispersion
Gold nano particle colloidal sols, and it is spare as seed.
(6) it is molten that tris solution, chlorauric acid solution, the gold nano grain of 16 nanometers of above-mentioned (5) gained are pressed
Glue and ultra-pure water 4:1:20-0.16:The volume ratio of 75-94.84, by tris solution, chlorauric acid solution, above-mentioned
(5) gold nano particle colloidal sols of 16 nanometers of gained are added sequentially in boiling water；
(7) boiling is kept, is heated to reflux 1 hour postcooling to room temperature, that is, obtains water-soluble mono and disperses spherical 30-150
The gold nano particle colloidal sols of nanometer
Embodiment 1
Using ultra-pure water by sodium citrate and gold chloride be configured to respectively mass percent concentration be 1% sodium citrate it is molten
The chlorauric acid solution that liquid and mass percent concentration are 1%.
Use oil-based solvent (one kind in toluene, hexane, amylalcohol or enanthol) by amine (octadecylamine, octadecenyl amine simultaneously
Or one kind in quaternary ammonium salt) it is configured to the oily solution containing amine that molar concentration is 0.0001 mol/L.
By volume 3:1 ratio weighs 0.5 milliliter of 1.5 milliliters of sodium citrate solution and chlorauric acid solution respectively.
Twoport flask is fixed on warm table and 48 milliliters of ultra-pure water (chlorauric acid solution, sodium citrate solution is added
It is 1 with ultrapure water volume ratio:3:96) 100 degrees Celsius of reflux, are heated rapidly to；Boiling water is added in 0.5 milliliter of chlorauric acid solution
In；Then 1.5 milliliters of sodium citrate solutions are added in the boiling water containing gold chloride；Ensure that reaction total volume is 50 milliliters, protects
Boiling is held, after being heated to reflux half an hour, is cooled to room temperature, you can it is monodispersed spherical to obtain the water solubility that grain size is 16 nanometers
Gold nano particle colloidal sols.
By 16 nanometers of gold nano particle colloidal sols and oily solution containing amine 5:1 volume ratio weigh respectively 5 milliliters it is above-mentioned
Gold nano particle colloidal sols and 1 milliliter of oily solution containing amine, make it be thoroughly mixed, and acutely rock 3-10 minutes；Rock completion
Afterwards, whole liquid are poured out to beaker, stands 0.5-6 hours, waits for that upper oil phase is volatilized completely, i.e., can be obtained on water phase surface macro
See the closs packing gold nano grain monofilm of size.
The present embodiment can get the macro-size closs packing monofilm for the gold nano grain that individual particle size is 16 nanometers.
Embodiment 2
Required raw material trishydroxymethylaminomethane and gold chloride are configured to solution respectively using ultra-pure water, wherein three hydroxyl first
The molar concentration of base aminomethane solution is 0.1 mol/L, and the mass percent concentration of chlorauric acid solution is 1%；It uses simultaneously
Oil-based solvent (one kind in toluene, hexane, amylalcohol, enanthol etc.) is by amine (one in octadecylamine, octadecenyl amine, quaternary ammonium salt etc.
Kind) it is configured to the oily solution containing amine that molar concentration is 0.001 mol/L.
By volume 4:1:20 ratio weighs 2 milliliters of tris solution, 0.5 milli of chlorauric acid solution respectively
It rises and 16 nanometers of 10 milliliters of gold nano particle colloidal sols in embodiment 1.
Twoport flask is fixed on warm table and be added 37.5 milliliters ultra-pure water (tris solution,
The volume ratio of chlorauric acid solution, 16 nanometers of gold nano colloidal sol and ultra-pure water is 4:1:20:75) 100 degrees Celsius, are heated rapidly to
Reflux；0.5 milliliter of chlorauric acid solution is added in boiling water；Then by 2 milliliters of tris solutions and 10 milliliters
16 nanometers of gold nano colloidal sol sequentially adds in the boiling water containing gold chloride；Ensure that reaction total volume is 50 milliliters, keep boiling,
It after being heated to reflux half an hour, is cooled to room temperature, you can obtain the monodispersed spherical gold nano of water solubility that grain size is 30 nanometers
Particle colloidal sols.
By gold nano particle colloidal sols and oily solution containing amine 5:3 volume ratio weighs 5 milliliters of above-mentioned gold nanos respectively
Particle colloidal sols and 3 milliliters of oily solutions containing amine, make it be thoroughly mixed, and acutely rock 3-10 minutes；It, will be complete after the completion of rocking
Portion's liquid is poured out to beaker, is stood 0.5-6 hours, is waited for that upper oil phase is volatilized completely, i.e., macro-size can be obtained on water phase surface
Closs packing gold nano grain monofilm.
The present embodiment can get the macro-size closs packing monofilm for the gold nano grain that individual particle size is 30 nanometers.
Embodiment 3
The present embodiment difference from Example 2 be the dosage of the gold nano colloidal sol of ultra-pure water and 16 nanometers be 46 milliliters and
1.5 milliliters, make tris solution, chlorauric acid solution, 16 nanometers of gold nano colloidal sol and the volume ratio of ultra-pure water
It is 4:1:3:92 (2 milliliters, 0.5 milliliter, 1.5 milliliters and 46 milliliters).The configuration molar concentration of oily solution containing amine is rubbed for 0.05
You/liter.
By gold nano particle colloidal sols and oily solution containing amine 5:2 volume ratio weighs 5 milliliters of above-mentioned gold nanos respectively
Particle colloidal sols and 2 milliliters of oily solutions containing amine, make it be thoroughly mixed,
Remaining condition is same as Example 2, can get the macroscopical ruler for the gold nano grain that individual particle size is 60 nanometers
Very little closs packing monofilm, transmission electron microscope photo are as shown in Figure 1.
Embodiment 4
The present embodiment difference from Example 2 is that the dosage of the gold nano colloidal sol of ultra-pure water and 16 nanometers is 47.05 millis
Rise and 0.45 milliliter, make tris solution, chlorauric acid solution, 16 nanometers of gold nano colloidal sol and the body of ultra-pure water
Product is than being 4:1:0.9:94.1 (2 milliliters, 0.5 milliliter, 0.45 milliliter and 47.05 milliliters).Configure oily solution containing amine mole
A concentration of 0.01 mol/L.
Remaining condition is same as Example 2, and the present embodiment can get the gold nano grain that individual particle size is 85 nanometers
Macro-size closs packing monofilm.
Embodiment 5
The present embodiment difference from Example 2 is that the dosage of the gold nano colloidal sol of ultra-pure water and 16 nanometers is 47.2 milliliters
With 0.3 milliliter, make tris solution, chlorauric acid solution, 16 nanometers of gold nano colloidal sol and the volume of ultra-pure water
Than being 4:1:0.6:94.4 (2 milliliters, 0.5 milliliter, 0.3 milliliter and 47.2 milliliters).Configure the molar concentration of oily solution containing amine
For 0.1 mol/L.
Remaining condition is same as Example 2, and the present embodiment can get the gold nano grain that individual particle size is 100 nanometers
Macro-size closs packing monofilm.
Embodiment 6
The present embodiment difference from Example 2 is that the dosage of the gold nano colloidal sol of ultra-pure water and 16 nanometers is 47.42 millis
Rise and 0.08 milliliter, make tris solution, chlorauric acid solution, 16 nanometers of gold nano colloidal sol and the body of ultra-pure water
Product is than being 4:1:0.16:94.84 (2 milliliters, 0.5 milliliter, 0.08 milliliter and 47.42 milliliters).Configuration oily solution containing amine rubs
A concentration of 0.1 mol/L of that.
Remaining condition is same as Example 2, and the present embodiment can get the gold nano grain that individual particle size is 150 nanometers
Macro-size closs packing monofilm.
Embodiment 7
With the closs packing gold nano for the macro-size that the individual particle size of nanometer gold grain that embodiment 3 obtains is 60 nanometers
For grain monofilm, carry out choosing Raman test specification.
Required p-aminophenyl thiophenol is configured to solution using absolute ethyl alcohol, molar concentration is 0.0001 mol/L.
It repeats to prepare in embodiment 3 and the step of self assembly, waits for that upper oil phase is volatilized completely, water phase surface can in beaker
Obtain macro-size auri self-assembled monolayer solid matter nanometer film.It is impregnated respectively using new configuration chloroazotic acid and saturation sodium hydroxide solution
Substrate (sheet glass, silicon chip or flexible substrates) 0.8-1.2 hours carries out soda acid processing, using soda acid treated substrate from beaker
Go deep into beaker at the one of interior no film, and by behind 45 degree of angles of substrate tilt close to nanometer film.After nanometer film and substrate have contact,
Slowly lifting substrate.The substrate surface removed from water phase can one layer of gold nano film of automatic load.Continue slowly lifting substrate, until
Film is completely pulled out.Then the substrate surface for being loaded with gold nano film is rinsed using ethyl alcohol, is placed under vacuum or nitrogen atmosphere
It is dry, it is spare in triplicate.
Substrate after thorough be cleaned and dried is soaked in the ethanol solution 1 hour of p-aminophenyl thiophenol, then uses nothing
Water-ethanol, which rinses, is loaded with the substrate surface of gold nano film, be placed under vacuum or nitrogen atmosphere it is dry, in triplicate after, carry out
The Raman test of random constituency.
The closs packing gold nano for the macro-size that the individual particle size of nanometer gold grain that the present embodiment obtains is 60 nanometers
The transmission electron microscope photo of grain monofilm is as shown in Figure 1；The random constituency Surface Enhanced Raman Scattering Spectrum such as Fig. 2 (a-c) of three of them
It is shown.Show that prepared macro-size, closely packed gold nano grain monofilm there can be uniform Raman signal, to real
Quantitative detection in their existing Raman enhancing fields.
Claims (7)
1. a kind of preparation method of the closs packing gold nano grain monofilm for the macro-size can be used as Raman enhancing substrate, special
Sign is：Include the following steps：
(1) 16 nanometers of gold nano particle colloidal sols are prepared, and prepare the Jenner of 30-150 nanometers of size range using it as seed
Rice grain colloidal sol；
(2) amine is configured to the oily solution containing amine that molar concentration is 0.0001-0.1 mol/Ls using oil-based solvent；
(3) gold nano particle colloidal sols are pressed with oily solution containing amine with 5:The volume ratio of 1-3 is thoroughly mixed, and is acutely rocked；
(4) it stands, waits for upper oil phase volatilization completely to get to the closs packing gold nano grain monofilm of macro-size；
(5) soda acid treated substrate is used, film is completely pulled out, after rinsing surface with absolute ethyl alcohol, in vacuum or nitrogen gas
It is dry under atmosphere.
2. the preparation method of macro-size closs packing gold nano grain monofilm according to claim 1, it is characterized in that：Institute
The preparation process for stating 16 nanometers of gold nano particle colloidal sols in step (1) is as described below：
1. sodium citrate and gold chloride are configured to the sodium citrate solution that mass percent concentration is 1% respectively using ultra-pure water
The chlorauric acid solution for being 1% with mass percent concentration；
2. by chlorauric acid solution and ultra-pure water 1:Chlorauric acid solution is added in boiling water by 96 volume ratio；
3. by sodium citrate solution and chlorauric acid solution 3:Sodium citrate solution is added step and 2. contains chlorine gold by 1 volume ratio
In the boiling water of acid, become boiling mixed liquor；
4. keeping boiling, 1 hour postcooling is heated to reflux to room temperature, that is, is obtained water-soluble mono and disperseed spherical 16 nanometers of Jenner
Rice grain colloidal sol.
3. the preparation method of macro-size closs packing gold nano grain monofilm according to claim 1, it is characterized in that：Institute
The preparation process for stating the gold nano particle colloidal sols that 30-150 nanometers of size range is prepared in step (1) is as described below：
1. trishydroxymethylaminomethane is configured to the trihydroxy methyl amino first that molar concentration is 0.1 mol/L using ultra-pure water
Alkane solution；Gold chloride is configured to the chlorauric acid solution that mass percent concentration is 1% using ultra-pure water；
2. pressing tris solution, chlorauric acid solution, 16 nanometers of gold nano particle colloidal sols and ultra-pure water 4:1:20-
0.16:The volume ratio of 75-94.84, tris solution, chlorauric acid solution, 16 nanometers of gold nano grain is molten
Glue is added sequentially in boiling water；
3. keeping boiling, 1 hour postcooling is heated to reflux to room temperature, that is, is obtained water-soluble mono and disperseed spherical 30-150 nanometers
Gold nano particle colloidal sols.
4. the preparation method of macro-size closs packing gold nano grain monofilm according to claim 1, it is characterized in that：Institute
It is toluene, hexane, amylalcohol or enanthol to state oil-based solvent.
5. the preparation method of macro-size closs packing gold nano grain monofilm according to claim 1, it is characterized in that：Institute
It is octadecylamine, octadecenyl amine or quaternary ammonium salt to state amine.
6. the preparation method of macro-size closs packing gold nano grain monofilm according to claim 1, it is characterized in that：Institute
Stating the detailed process of step (5) is：
Soda acid processing is carried out to substrate, using soda acid treated substrate without going deep into beaker from film out of beaker, and by beaker
Close to nanometer film behind 45 degree of angles of inclination；After nanometer film and substrate have contact, substrate is slowly lifted, until film is completely pulled out；
Then the substrate surface for being loaded with gold nano film is rinsed using absolute ethyl alcohol, is placed under vacuum or nitrogen atmosphere dry.
7. the preparation method of macro-size closs packing gold nano grain monofilm according to claim 6, it is characterized in that：Institute
It states and refers to substrate progress soda acid processing：Respectively substrate, time are impregnated using new configuration chloroazotic acid and saturation sodium hydroxide solution
0.8-1.2 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810590635.XA CN108526487B (en) | 2018-06-09 | 2018-06-09 | A kind of preparation method of macro-size closs packing gold nano grain monofilm |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810590635.XA CN108526487B (en) | 2018-06-09 | 2018-06-09 | A kind of preparation method of macro-size closs packing gold nano grain monofilm |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108526487A true CN108526487A (en) | 2018-09-14 |
| CN108526487B CN108526487B (en) | 2019-07-30 |
Family
ID=63470759
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810590635.XA Active CN108526487B (en) | 2018-06-09 | 2018-06-09 | A kind of preparation method of macro-size closs packing gold nano grain monofilm |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108526487B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109834292A (en) * | 2019-04-11 | 2019-06-04 | 中国科学院宁波材料技术与工程研究所 | Macroscopical large-area two-dimensional Janus nano-gold film and the preparation method and application thereof |
| CN110261367A (en) * | 2019-07-10 | 2019-09-20 | 中国科学技术大学 | A kind of SERS substrate, preparation method, regulate and control SERS substrate hotspot architecture method and SERS substrate application |
| CN112683419A (en) * | 2020-12-21 | 2021-04-20 | 山东大学 | Method for accurately detecting temperature based on surface enhanced Raman scattering effect |
| CN113277546A (en) * | 2021-04-15 | 2021-08-20 | 蚌埠学院 | Preparation method of gold nanoparticle implanted three-dimensional zinc oxide nano network material |
| CN115582537A (en) * | 2022-10-08 | 2023-01-10 | 温州医科大学 | Preparation method and application of large-size uniform nano noble metal film |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103590037A (en) * | 2013-11-20 | 2014-02-19 | 苏州大学 | Gold nanoparticle monofilm preparation method and device thereof |
| CN104614361A (en) * | 2015-01-21 | 2015-05-13 | 中国科学院合肥物质科学研究院 | SERS (surface-enhanced Raman spectrum) detection method for narcotics in urine sample |
| CN105115958A (en) * | 2015-09-17 | 2015-12-02 | 苏州大学 | Surface-enhanced Raman substrate based on large-sized metal nanoparticles and preparation method thereof |
| CN105252016A (en) * | 2015-11-11 | 2016-01-20 | 西安电子科技大学 | Preparation method of gold nanoparticle self-assembled transplantable single-layer thin film |
| CN105954251A (en) * | 2016-04-07 | 2016-09-21 | 南京邮电大学 | Surface enhanced Raman scattering substrate and manufacturing method thereof |
| CN106770175A (en) * | 2017-01-19 | 2017-05-31 | 上海海洋大学 | A kind of method that utilization SERS detects paraquat |
| CN107243626A (en) * | 2017-04-05 | 2017-10-13 | 厦门稀土材料研究所 | The synthesis of Silver nanorod and based on its prepare Raman spectrum base |
| CN107746468A (en) * | 2017-11-01 | 2018-03-02 | 中国科学院城市环境研究所 | A kind of self-supporting nanometer assembled material and preparation method thereof |
-
2018
- 2018-06-09 CN CN201810590635.XA patent/CN108526487B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103590037A (en) * | 2013-11-20 | 2014-02-19 | 苏州大学 | Gold nanoparticle monofilm preparation method and device thereof |
| CN104614361A (en) * | 2015-01-21 | 2015-05-13 | 中国科学院合肥物质科学研究院 | SERS (surface-enhanced Raman spectrum) detection method for narcotics in urine sample |
| CN105115958A (en) * | 2015-09-17 | 2015-12-02 | 苏州大学 | Surface-enhanced Raman substrate based on large-sized metal nanoparticles and preparation method thereof |
| CN105252016A (en) * | 2015-11-11 | 2016-01-20 | 西安电子科技大学 | Preparation method of gold nanoparticle self-assembled transplantable single-layer thin film |
| CN105954251A (en) * | 2016-04-07 | 2016-09-21 | 南京邮电大学 | Surface enhanced Raman scattering substrate and manufacturing method thereof |
| CN106770175A (en) * | 2017-01-19 | 2017-05-31 | 上海海洋大学 | A kind of method that utilization SERS detects paraquat |
| CN107243626A (en) * | 2017-04-05 | 2017-10-13 | 厦门稀土材料研究所 | The synthesis of Silver nanorod and based on its prepare Raman spectrum base |
| CN107746468A (en) * | 2017-11-01 | 2018-03-02 | 中国科学院城市环境研究所 | A kind of self-supporting nanometer assembled material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| ZHANG, PEINA ETAL: "High-Yield Production of Uniform Gold Nanoparticles with Sizes from 31 to 577 nm via One-Pot Seeded Growth and Size-Dependent SERS Property", 《PARTICLE & PARTICLE SYSTEMS CHARACTERIZATION》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109834292A (en) * | 2019-04-11 | 2019-06-04 | 中国科学院宁波材料技术与工程研究所 | Macroscopical large-area two-dimensional Janus nano-gold film and the preparation method and application thereof |
| CN109834292B (en) * | 2019-04-11 | 2021-11-23 | 中国科学院宁波材料技术与工程研究所 | Macroscopic large-area two-dimensional Janus nano gold film and preparation method and application thereof |
| CN110261367A (en) * | 2019-07-10 | 2019-09-20 | 中国科学技术大学 | A kind of SERS substrate, preparation method, regulate and control SERS substrate hotspot architecture method and SERS substrate application |
| CN112683419A (en) * | 2020-12-21 | 2021-04-20 | 山东大学 | Method for accurately detecting temperature based on surface enhanced Raman scattering effect |
| CN112683419B (en) * | 2020-12-21 | 2021-12-24 | 山东大学 | Method for accurately detecting temperature based on surface enhanced Raman scattering effect |
| CN113277546A (en) * | 2021-04-15 | 2021-08-20 | 蚌埠学院 | Preparation method of gold nanoparticle implanted three-dimensional zinc oxide nano network material |
| CN115582537A (en) * | 2022-10-08 | 2023-01-10 | 温州医科大学 | Preparation method and application of large-size uniform nano noble metal film |
| CN115582537B (en) * | 2022-10-08 | 2023-05-16 | 温州医科大学 | Preparation method and application of large-size uniform nano noble metal film |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108526487B (en) | 2019-07-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108526487B (en) | A kind of preparation method of macro-size closs packing gold nano grain monofilm | |
| Hussain et al. | Size-controlled synthesis of near-monodisperse gold nanoparticles in the 1− 4 nm range using polymeric stabilizers | |
| Su et al. | A reproducible SERS substrate based on electrostatically assisted APTES-functionalized surface-assembly of gold nanostars | |
| Sweeney et al. | Rapid purification and size separation of gold nanoparticles via diafiltration | |
| Nithiyanantham et al. | Self-assembled wire-like and honeycomb-like osmium nanoclusters (NCs) in DNA with pronounced catalytic and SERS activities | |
| Bechelany et al. | Simple synthetic route for SERS-active gold nanoparticles substrate with controlled shape and organization | |
| Gou et al. | A highly effective electrochemical chiral sensor of tryptophan enantiomers based on covalently functionalize reduced graphene oxide with L-lysine | |
| Karimizefreh et al. | Impedimetic biosensor for the DNA of the human papilloma virus based on the use of gold nanosheets | |
| Gu et al. | Facile fabrication of a silver dendrite-integrated chip for surface-enhanced Raman scattering | |
| CN104607657B (en) | Copper-silver double-metal nanowire and preparation method thereof | |
| CN105965029B (en) | The synthetic method of water-soluble monodispersed spherical gold-silver alloy nano particle | |
| Jiang et al. | Silver nanocube-mediated sensitive immunoassay based on surface-enhanced Raman scattering assisted by etched silicon nanowire arrays | |
| CN107322004A (en) | A kind of silver/redox graphene nano composite material and application | |
| Roy et al. | Silver nanoflowers for single-particle SERS with 10 pM sensitivity | |
| Mhlanga et al. | Fabrication of surface enhanced Raman spectroscopy substrates on solid supports | |
| Dou et al. | An ultrasensitive, disposable, and “plug and play” surface-enhanced raman scattering substrate for the in situ detection of trace thiram in water | |
| CN109030456A (en) | A kind of Surface enhanced Raman spectroscopy detection substrate and its preparation method and application | |
| Deschaume et al. | Synthesis and properties of gold nanoparticle arrays self-organized on surface-deposited lysozyme amyloid scaffolds | |
| CN111856012A (en) | Method for detecting cancer antigen 125 based on up-conversion nano material and carbon quantum dot fluorescence resonance energy transfer | |
| Li et al. | Surface enhanced Raman scattering properties of dynamically tunable nanogaps between Au nanoparticles self-assembled on hydrogel microspheres controlled by pH | |
| Melo et al. | Microwires of Au–Ag nanocages patterned via magnetic nanoadhesives for investigating proteins using surface enhanced infrared absorption spectroscopy | |
| CN104330397A (en) | Surface enhanced Raman scattering substrate with ordered crystal structure and application of surface enhanced Raman scattering substrate | |
| Peng et al. | Fabrication of high-performance microfluidic SERS substrates by metal-assisted chemical etching of silicon scratches | |
| KR102067888B1 (en) | ELECTROCHEMICAL SENSOR DETECTING NITROBENZENE USING Au-Ag ALLOY NANODOTS AND METHOD OF THE SAME | |
| CN104841945B (en) | A kind of large scale silver thin slice and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |