CN114226743B - Preparation method of island film-shaped nano cubic array structure - Google Patents
Preparation method of island film-shaped nano cubic array structure Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000011258 core-shell material Substances 0.000 claims abstract description 65
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 57
- 239000010703 silicon Substances 0.000 claims abstract description 57
- PQTCMBYFWMFIGM-UHFFFAOYSA-N gold silver Chemical compound [Ag].[Au] PQTCMBYFWMFIGM-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000000758 substrate Substances 0.000 claims abstract description 46
- 238000001704 evaporation Methods 0.000 claims abstract description 29
- 230000008020 evaporation Effects 0.000 claims abstract description 26
- 239000000523 sample Substances 0.000 claims abstract description 17
- 238000000151 deposition Methods 0.000 claims abstract description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 46
- 229910052737 gold Inorganic materials 0.000 claims description 44
- 239000010931 gold Substances 0.000 claims description 44
- 238000000034 method Methods 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 24
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000011668 ascorbic acid Substances 0.000 claims description 11
- 229960005070 ascorbic acid Drugs 0.000 claims description 11
- 235000010323 ascorbic acid Nutrition 0.000 claims description 11
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 7
- 239000012279 sodium borohydride Substances 0.000 claims description 7
- 239000013078 crystal Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- 108010011485 Aspartame Proteins 0.000 claims description 3
- IAOZJIPTCAWIRG-QWRGUYRKSA-N aspartame Chemical compound OC(=O)C[C@H](N)C(=O)N[C@H](C(=O)OC)CC1=CC=CC=C1 IAOZJIPTCAWIRG-QWRGUYRKSA-N 0.000 claims description 3
- 229960003438 aspartame Drugs 0.000 claims description 3
- 235000010357 aspartame Nutrition 0.000 claims description 3
- 239000000605 aspartame Substances 0.000 claims description 3
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 7
- 238000001237 Raman spectrum Methods 0.000 abstract description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical group [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 229910052709 silver Chemical group 0.000 description 10
- 239000004332 silver Chemical group 0.000 description 10
- 239000002356 single layer Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 6
- 238000001338 self-assembly Methods 0.000 description 6
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 101000674278 Homo sapiens Serine-tRNA ligase, cytoplasmic Proteins 0.000 description 3
- 101000674040 Homo sapiens Serine-tRNA ligase, mitochondrial Proteins 0.000 description 3
- 102100040516 Serine-tRNA ligase, cytoplasmic Human genes 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 229910004042 HAuCl4 Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
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- 239000007769 metal material Substances 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- 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
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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Abstract
The application relates to a preparation method of an island-film-shaped nano cubic array structure, in particular to the field of nano cubic array structures. The application provides a preparation method of an island film-shaped nano cubic array structure, which comprises the following steps: a preset substrate is arranged in a first container, a preset silicon wafer is arranged on the preset substrate, gold-silver core-shell nano cubic sol is arranged on the surface of the preset silicon wafer, and a second container is covered on the preset substrate; the application controls the temperature or humidity of the gold-silver core-shell nano cubic sol to make the evaporation rate of the gold-silver core-shell nano cubic sol close to that of the edge position, thereby avoiding the coffee ring effect and depositing the preset probe molecules on the surface of the island-film nano cubic array structure; the probe molecules are preset, so that the island-film-shaped nano cubic array structure can detect the Raman spectrum intensity.
Description
Technical Field
The application relates to the field of nano cubic array structures, in particular to a preparation method of an island film-shaped nano cubic array structure.
Background
In recent years, noble metal nanostructures have received attention because of the many interesting optical properties they produce when excited under specific excitation conditions. Particularly, with the development of application physics, the metal material with the nanostructure is widely applied to the fields of surface plasmons, biomedical treatment, photoelectric detection and the like.
The self-assembly is to form a long-term stable and ordered structure by specific interaction of nano particles existing in a disturbance system, and different self-assembly modes not only can directly change the arrangement mode of noble metal particles on a substrate, but also can indirectly influence the local electromagnetic field distribution and strength of a substrate under specific excitation, so that the enhancement effect of the structure on molecular Raman signals is different. The current self-assembly methods for nanoparticles include gas-liquid, liquid-liquid, evaporation, electric field, centrifugal force, magnetic field, optical regulation and control, and the like.
In the prior art, in the self-assembly process, due to the concentration difference formed by the surfactant, a coffee ring effect is formed on the surface of the noble metal nano structure, namely, under the natural evaporation of the colloidal solution, the evaporation rate of the edge of the liquid drop is far greater than that of the central solution of the liquid drop, so that the capillary action of one edge direction in the liquid drop can be caused, and meanwhile, the solute can be continuously brought to the edge of the liquid drop and deposited continuously, so that the self-assembly process is finally formed.
Disclosure of Invention
The application aims to overcome the defects in the prior art, and provides a preparation method of an island-film-shaped nano cubic array structure, which aims to solve the problems that in the prior art, a coffee ring effect is formed on the surface of a noble metal nano structure due to concentration difference formed by a surfactant, namely, under natural evaporation of a colloid solution, the evaporation rate of the edge of a liquid drop is far greater than that of a liquid drop center solution, so that capillary action of one edge inside the liquid drop is caused, and solute is continuously brought to the edge of the liquid drop and is continuously deposited, and finally the problem is formed.
In order to achieve the above purpose, the technical scheme adopted by the embodiment of the application is as follows:
in a first aspect, the present application provides a method for preparing an island-film-shaped nanocube array structure, the method comprising:
a preset substrate is arranged in a first container, a preset silicon wafer is arranged on the preset substrate, gold-silver core-shell nano-cubic sol is arranged on the surface of the preset silicon wafer, and a second container is used for covering the preset substrate, wherein the gold-silver core-shell nano-cubes are of a core-shell structure of silver-cube coated gold balls;
injecting preset liquid between a first container and a second container, and controlling the evaporation rate of the second container so that the gold-silver core-shell nano cubic sol forms an island film-shaped nano cubic array structure on a preset silicon wafer;
and depositing preset probe molecules on the surface of the island-film-shaped nano cubic array structure.
Optionally, the preset substrate is disposed inside the first container, the preset silicon wafer is disposed on the preset substrate, the gold-silver core-shell nano cubic sol is disposed on the surface of the preset silicon wafer, and before the step of reversely buckling the second container on the preset substrate, the method further comprises:
preparing a gold seed solution by using chloroauric acid, sodium borohydride and cetyltrimethylammonium bromide;
pouring chloroauric acid, ascorbic acid and hexadecyl trimethyl ammonium chloride into a gold seed solution to generate gold ball sol;
sequentially adding silver nitrate, ascorbic acid solution and hexadecyl trimethyl ammonium chloride into gold ball sol, and generating gold-silver core-shell nano cubic sol in the gold ball sol.
Optionally, the step of preparing the seed solution using chloroauric acid, sodium borohydride, cetyltrimethylammonium bromide further comprises:
cleaning the surface of the preset silicon wafer in an ultrasonic environment for 2-8 minutes by using an acetone solution;
cleaning the surface of the preset silicon wafer in an ultrasonic environment for 2-5 minutes by using an ethanol solution;
washing the surface of the preset silicon wafer in an ultrasonic environment by using deionized water for 5-10 minutes;
and setting the preset silicon wafer in an oven for drying.
Optionally, the step of injecting the preset liquid between the first container and the second container and controlling the evaporation rate of the second container to form the island-film-shaped nano cubic array structure on the preset silicon wafer by using the gold-silver core-shell nano cubic sol specifically comprises the following steps:
injecting a predetermined liquid between the first container and the second container;
the evaporation rate of the central position and the edge position of the gold-silver core-shell nano cubic sol is changed by controlling the environmental temperature of the second container and/or controlling the humidity in the second container;
and (3) evaporating the gold-silver core-shell nano cubic sol to form an island film-shaped nano cubic array structure on a preset silicon wafer.
Optionally, the preset probe molecule comprises rhodamine and any one of crystal violet and aspartame.
Optionally, the ratio of the bottom areas of the first container and the second container is 2:1-3:1.
Alternatively, the first container has a volume of 400ml to 600ml and the second container has a volume of 100ml to 300ml.
The beneficial effects of the application are as follows:
the application provides a preparation method of an island film-shaped nano cubic array structure, which comprises the following steps: a preset substrate is arranged in a first container, a preset silicon wafer is arranged on the preset substrate, gold-silver core-shell nano-cubic sol is arranged on the surface of the preset silicon wafer, and a second container is used for covering the preset substrate, wherein the gold-silver core-shell nano-cubes are of a core-shell structure of silver-cube coated gold balls; injecting preset liquid between a first container and a second container, and controlling the evaporation rate in the second container so that the gold-silver core-shell nano cubic sol forms an island film-shaped nano cubic array structure on a preset silicon wafer; the application controls the temperature or humidity of the gold-silver core-shell nano cubic sol to make the evaporation rate of the gold-silver core-shell nano cubic sol close, and the solute concentration gradient difference and the surface tension difference of the two positions can generate central acting force, thereby solving the problem of coffee ring effect to a certain extent and depositing preset probe molecules on the surface of the island-film nano cubic array structure; the preset probe molecules can enable the island film-shaped nano cubic array structure to detect the Raman spectrum intensity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method for fabricating an island-film-shaped nanocube array structure according to an embodiment of the present application;
FIG. 2 is a flowchart of a method for fabricating an island-film-shaped nanocube array structure according to an embodiment of the present application;
FIG. 3 is a flowchart of a method for fabricating an island-film-shaped nanocube array structure according to an embodiment of the present application;
FIG. 4 is a flowchart of a method for fabricating an island-film-shaped nanocube array structure according to an embodiment of the present application;
fig. 5 is a physical diagram and an SEM diagram of a single-layer island-film-shaped gold-silver core-shell nanocube array substrate prepared in this example;
fig. 6 is a diagram showing the uniformity verification of the single-layer island film-shaped gold-silver core-shell nanocube array substrate prepared in this example.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are one embodiment of the present application, but not all embodiments. The components of the embodiments of the present application generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
In order to make the implementation of the present application more clear, the following detailed description will be given with reference to the accompanying drawings.
FIG. 1 is a flow chart of a method for fabricating an island-film-shaped nanocube array structure according to an embodiment of the present application; as shown in fig. 1, the application provides a preparation method of an island film-shaped nano cubic array structure, which comprises the following steps:
s101, setting a preset substrate in a first container, setting a preset silicon wafer on the preset substrate, setting gold-silver core-shell nano cubic sol on the surface of the preset silicon wafer, and covering the preset substrate by using a second container.
The devices used in the method of the application respectively comprise: the method comprises the steps of a first container, a second container, a preset silicon wafer, gold and silver core-shell nano cubic sol and a preset substrate, wherein the first container is a container with larger bottom area, the second container is a container with smaller bottom area, the preset silicon wafer is in a pre-cut shape, in practical application, the preset silicon wafer is rectangular, the preset substrate is made of materials according to practical requirements, the preset substrate is smooth in surface and difficult to absorb water and difficult to breathe, in practical application, the preset substrate is arranged in the first beaker, the preset silicon wafer is arranged above the preset substrate, the gold and silver core-shell nano cubic sol is arranged on the preset silicon wafer, the second beaker is covered outside the preset substrate, the preset silicon wafer, the gold and silver core-shell nano cubic sol and the preset substrate are covered, and in practical application, the gold and silver core-shell nano cubic sol is a sol material, the gold and silver core-shell nano cubic sol is a gold core, and a silver core-shell nano cubic structure is wrapped outside the gold core-shell nano cubic sol, and is not limited by the practical requirements, and the specific container is arranged at the first container to the second container 1, and the specific container 1 to the specific container is not limited by the practical requirements. Alternatively, the first container has a volume of 400ml to 600ml and the second container has a volume of 100ml to 300ml. In practical application, the volume of the first container is generally selected to be 500ml, and the volume of the second container is generally selected to be 200ml, wherein the gold-silver core-shell nanocubes are core-shell structures of silver-cube coated gold balls.
S102, injecting preset liquid between the first container and the second container, and controlling the evaporation rate of the second container, so that the gold-silver core-shell nano cubic sol forms an island film-shaped nano cubic array structure on a preset silicon wafer.
Because the bottom surface area and the volume of the first container are both larger than those of the second container, when the second container is covered inside the first container, a gap exists between the first container and the second container, preset liquid is injected between the first container and the second container, so that the inside of the second container is in a sealed state, the second container in the sealed state can control the evaporation rate of the gold-silver core-shell nano-cubic sol inside the second container by controlling the outside temperature, generally, the higher the temperature is, the faster the evaporation rate of the gold-silver core-shell nano-cubic sol is, in addition, the second container is covered inside the first container, the preset amount of water vapor is injected inside the second container, the humidity inside the second container is changed, the evaporation rate of the gold-silver core-shell nano-cubic sol inside the second container is also changed, in practical application, the two methods for controlling the evaporation rate of the second container can be simultaneously applied, the gold-silver core-shell nano-cubic sol with specific concentration is under specific temperature and humidity conditions, the gold-silver core-shell nano-cubic sol is slowly evaporated, and the gradient of the gold-silver core-shell nano-cubic sol is formed at the center of a certain gradient, and the gradient of the gold-silver core-shell nano-cubic sol is formed at the center of a certain gradient, and the gradient of the gold-shell nano-cubic sol is formed at the center of a certain position, and the gradient of a film-like particle array is further, and the gradient of the gradient is avoided.
FIG. 2 is a flowchart of a method for fabricating an island-film-shaped nanocube array structure according to an embodiment of the present application; as shown in fig. 2; optionally, the step of injecting the preset liquid between the first container and the second container and controlling the evaporation rate of the second container to form the island-film-shaped nano cubic array structure on the preset silicon wafer by using the gold-silver core-shell nano cubic sol specifically comprises the following steps:
s201, injecting a preset liquid between the first container and the second container.
The preset liquid is injected between the first container and the second container, the preset liquid is selected according to actual needs, the preset liquid is not particularly limited herein, for convenience of explanation, the preset liquid is used as water, and the water is arranged between the first container and the second container, so that the liquid seal of the second container is realized.
S202, changing the evaporation rate of the central position and the edge position of the gold-silver core-shell nano cubic sol by controlling the ambient temperature of the second container and/or controlling the humidity inside the second container.
The method can independently change the evaporation rate of the central position and the edge position of the gold-silver core-shell nano cubic sol by controlling the ambient temperature of the second container, can also change the evaporation rate of the central position and the edge position of the gold-silver core-shell nano cubic sol by controlling the humidity inside the second container, can also change the evaporation rate of the central position and the edge position of the gold-silver core-shell nano cubic sol by simultaneously controlling the ambient temperature of the second container and controlling the humidity inside the second container, and is particularly controlled according to the actual requirement, and is not particularly limited herein, generally, the larger the humidity inside the second container is, the larger the evaporation rate of the gold-silver core-shell nano cubic sol inside the second container is, the higher the temperature outside the second container is, and the larger the evaporation rate of the gold-silver core-shell nano cubic sol inside the second container is; in practical application, the temperature of the second container is controlled by cooling or heating the second container through a temperature control device.
S203, evaporating the gold-silver core-shell nano cubic sol to form an island film-shaped nano cubic array structure on a preset silicon wafer.
The constant temperature and humidity in the small beaker are controlled through the incubator, so that the gold and silver core-shell nano cubic sol with specific concentration is evaporated to form an island film-shaped nano cubic array structure on a preset silicon wafer, namely a tiled single-layer film structure, and nano particles in the solution are closely arranged one by one to form an island film-shaped array substrate. The nano particles are of a core-shell structure of a cubic coated sphere with external silver and internal gold, the outlines of the corners of the cubes are clear, the appearance is uniform, and the overall size is about 45nm.
S103, depositing preset probe molecules on the surface of the island-film-shaped nano cubic array structure.
The preset probe molecules comprise rhodamine, crystal violet and aspartame, wherein the preset probe molecules are used for detecting Raman spectra, the peak positions of the plurality of preset probe molecules are different, so that the intensity of the Raman spectra is enhanced, and when the Raman spectra are detected, the preset probe molecules enhance Raman signals, so that the Raman spectra are easier to observe.
FIG. 3 is a flowchart of a method for fabricating an island-film-shaped nanocube array structure according to an embodiment of the present application; as shown in fig. 3; optionally, the preset substrate is disposed inside the first container, the preset silicon wafer is disposed on the preset substrate, the gold-silver core-shell nano cubic sol is disposed on the surface of the preset silicon wafer, and before the step of reversely buckling the second container on the preset substrate, the method further comprises:
s301, preparing a gold seed solution by using chloroauric acid, sodium borohydride and cetyltrimethylammonium bromide.
In a beaker, adding 10ml of CTAB solution with the concentration of 0.1M, 0.25ml of HAuCl4 solution with the concentration of 0.01M and 0.6ml of NaBH4 solution with the concentration of 0.01M into the beaker in sequence to react to generate gold seed solution, namely, gold particles are used as solutes in the solution.
S302, pouring chloroauric acid, ascorbic acid and hexadecyl trimethyl ammonium chloride into the gold seed solution to generate gold ball sol.
Into a beaker were successively added 2ml of CTAC solution at a concentration of 0.2M, 2ml of HAuCl at a concentration of 0.5mM 4 The gold seed solution is firstly grown into gold ball sol with the diameter of 8-10nm, and then reacts to generate gold seed solution which is grown into gold ball sol with the diameter of 8-10nm, and compared with the gold seed solution, the gold ball solution has the radius of solute which is far larger than that of the gold seed solution. Alternatively, 25ml of CTAC solution at a concentration of 0.1M, 1.625ml of AA solution at a concentration of 0.1M, 0.7ml of 10nm gold ball sol, 25ml of HAuCl at a concentration of 0.5mM are sequentially added to a standard beaker having a capacity of 50ml 4 The solution is used for enabling gold seed solution to grow into 18-28nm gold ball sol firstly. Alternatively, the reaction-completed sol sample was centrifuged at 8000rad for 15min to remove CTAC micelles from the solution and redispersed in 5ml of CTAC sol at 20 mM.
S303, sequentially adding silver nitrate, ascorbic acid solution and cetyltrimethylammonium chloride into the gold ball sol, and generating gold-silver core-shell nano cubic sol in the gold ball sol.
Sequentially adding silver nitrate, ascorbic acid solution and hexadecyl trimethyl ammonium chloride into the beaker, and reacting to obtain silver simple substance attached to the outside of the gold particles to form gold-silver core-shell nanocubes; in practical application, an ascorbic acid solution is also needed to be prepared firstly, wherein the specific flow is that one part of CTAC crystal has the amount of 0.8g, one part of ionized water has the amount of 2.5ml and can be prepared into a CTAB solution with the concentration of 0.1mol/L, one part of ascorbic acid crystal has the amount of 0.0123g, one part of ionized water has the amount of 7ml and is prepared into an ascorbic acid solution with the concentration of 0.01 mol/L; specifically, the process for generating gold-silver core-shell nano cubic sol in gold ball sol specifically comprises the following steps: into a standard beaker with a capacity of 50ml, 5ml of gold sphere sol with a 28nm concentration, 0.5ml of AgNO3 solution with a concentration of 50mM and 0.5ml of ascorbic acid sol with a concentration of 0.5M are sequentially added to obtain a core-shell structure of silver cube coated gold spheres. Alternatively, the reaction completed sol sample was centrifuged twice at 8500rad for 10min to remove CTAC micelles from the solution.
FIG. 4 is a flowchart of a method for fabricating an island-film-shaped nanocube array structure according to an embodiment of the present application; as shown in fig. 4; optionally, the step of preparing the seed solution using chloroauric acid, sodium borohydride, cetyltrimethylammonium bromide further comprises:
s401, cleaning the surface of the preset silicon wafer in an ultrasonic environment by using an acetone solution for 2-8 minutes.
Cleaning the surface of a preset silicon wafer by using an acetone solution, arranging the preset silicon wafer in the acetone solution, and ultrasonically vibrating for a period of time by using an ultrasonic instrument to remove dirt on the surface of the preset silicon wafer, wherein the preset silicon wafer is optionally cleaned by using the acetone solution for 2-8 minutes, and the cleaning time is selected according to actual needs and is not particularly limited.
S402, cleaning the surface of the preset silicon wafer in an ultrasonic environment for 2-5 minutes by using an ethanol solution.
After the preset silicon wafer is cleaned by using the acetone solution, the acetone solution and impurity dirt on the surface of the preset silicon wafer are further cleaned by using the ethanol solution, the preset silicon wafer is arranged in the ethanol solution, ultrasonic vibration is carried out for a period of time by using an ultrasonic instrument to remove the dirt on the surface of the preset silicon wafer, alternatively, the surface of the preset silicon wafer is cleaned by using the ethanol solution for 2 minutes to 5 minutes, the cleaning time is selected according to actual needs, and the cleaning time is not particularly limited herein
S403, cleaning the surface of the preset silicon wafer in an ultrasonic environment by using deionized water for 5-10 minutes.
The deionized water is used for cleaning the ethanol solution of the preset silicon wafer, the preset silicon wafer is arranged in the ionized water, ultrasonic vibration is carried out for a period of time by using an ultrasonic instrument to remove other solutions and dirt on the surface of the preset silicon wafer, optionally, the ionized water is used for cleaning the surface of the preset silicon wafer for 2 minutes to 5 minutes, and the cleaning time is selected according to actual needs and is not particularly limited.
S404, setting the preset silicon wafer in an oven for drying.
And (3) arranging the cleaned preset silicon wafer in an oven, and drying at 60 ℃.
The method has the beneficial effects that: the single-layer island film-shaped gold-silver core-shell nano-cube substrate can be obtained by evaporation self-assembly by controlling the volatilization rate of a solute only by changing the concentration of the sol dripped in the device and the temperature and humidity of the environment where a sample is positioned without adding additional reagents. The single-layer island film-shaped gold-silver core-shell nanocube substrate prepared by the method has excellent uniformity, cleanliness and stability, and can be applied to the fields of surface plasmons, biomedical treatment, photoelectric detection, nano electronic devices and the like. The method has the advantages of convenient operation and strong universality, and can lead the nanocubes to form the array substrate which is tightly arranged. The application can reduce the evaporation rate difference between the center and the edge by controlling the temperature and humidity in the device, and can eliminate the coffee ring effect due to the marangoni vortex formed by the concentration difference formed by the surfactant, and finally the single-layer island film-shaped gold-silver core-shell nanocube substrate is obtained by evaporating on the surface of the solid substrate.
Fig. 5 is a physical diagram and an SEM diagram of a single-layer island-film-shaped gold-silver core-shell nanocube array substrate prepared in this embodiment, and as shown in fig. 5, it can be seen that the mold is distributed in island shape, is closely arranged, has a regular structure, and has an array of nanocubes that are closely arranged.
Fig. 6 is a diagram for verifying uniformity of a single-layer island-film gold-silver core-shell nano-cubic array substrate prepared by the embodiment, and as shown in fig. 6, a confocal microscopic raman instrument is used for measuring raman scattering signals of preselected probe molecules deposited on the surface of a substrate structure, so that uniformity of the film under the nanoscale is characterized, and in 10 randomly selected areas, the SERS signals are consistent, and the substrate is proved to have higher SERS activity and good uniformity, and can be used as an excellent SERS substrate in the surface analysis and detection fields.
The above is only a preferred embodiment of the present application, and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (4)
1. The preparation method of the island membranous nano cubic array structure is characterized by comprising the following steps of:
a preset substrate is arranged in a first container, a preset silicon wafer is arranged on the preset substrate, gold-silver core-shell nano-cubic sol is arranged on the surface of the preset silicon wafer, and a second container is used for covering the preset substrate, wherein the gold-silver core-shell nano-cubes are of a core-shell structure of silver-cube coated gold balls, and the ratio of the bottom areas of the first container to the second container is 2:1-3:1;
injecting preset liquid between the first container and the second container, and controlling the evaporation rate of the second container by adjusting the temperature or humidity of the gold-silver core-shell nano cubic sol so that the gold-silver core-shell nano cubic sol forms an island film-shaped nano cubic array structure on the preset silicon wafer;
and depositing preset probe molecules on the surface of the island film-shaped nano cubic array structure.
2. The method for preparing an island-film nanocube array structure according to claim 1, wherein the step of arranging a preset substrate inside a first container, arranging a preset silicon wafer on the preset substrate, arranging gold-silver core-shell nanocube sol on the surface of the preset silicon wafer, and reversely buckling the preset substrate by using a second container further comprises:
preparing a gold seed solution by using chloroauric acid, sodium borohydride and cetyltrimethylammonium bromide;
pouring chloroauric acid, ascorbic acid and hexadecyl trimethyl ammonium chloride into the gold seed solution to generate gold ball sol;
sequentially adding silver nitrate, ascorbic acid solution and cetyltrimethylammonium chloride into the gold ball sol, and generating gold-silver core-shell nano cubic sol in the gold ball sol.
3. The method for preparing an island-film-shaped nanocube array structure according to claim 2, wherein the step of preparing a gold seed solution using chloroauric acid, sodium borohydride, cetyltrimethylammonium bromide further comprises:
cleaning the surface of the preset silicon wafer in an ultrasonic environment for 2-8 minutes by using an acetone solution;
using ethanol solution to clean the surface of the preset silicon wafer in an ultrasonic environment for 2-5 minutes;
washing the surface of the preset silicon wafer in an ultrasonic environment by using deionized water for 5-10 minutes;
and setting the preset silicon chip in an oven for drying.
4. The method for preparing an island-film-shaped nanocube array structure according to claim 1, wherein the preset probe molecules comprise rhodamine, crystal violet and aspartame.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102251286A (en) * | 2011-07-08 | 2011-11-23 | 中国科学院理化技术研究所 | Micron/nano cone array of germanium and preparation method thereof |
| CN103526291A (en) * | 2013-10-28 | 2014-01-22 | 中国工程物理研究院化工材料研究所 | Surface enhanced Raman scattering substrate, preparation method therefor and application thereof |
| CN104155284A (en) * | 2014-08-15 | 2014-11-19 | 中国工程物理研究院化工材料研究所 | ZnO-Ag surface enhanced Raman scattering chip, and making method, preserving method and use thereof |
| CN104404624A (en) * | 2014-11-28 | 2015-03-11 | 中国科学院合肥物质科学研究院 | Controllable preparation method of three-dimensional nano plasmon polariton super crystals |
| CN107101989A (en) * | 2017-03-16 | 2017-08-29 | 安徽中科赛飞尔科技有限公司 | Construction method based on Parameter adjustable control self-assembled structures substrate and its SERS detection methods for drugs |
| WO2018069646A1 (en) * | 2016-10-13 | 2018-04-19 | Universite Paris Diderot | Synthesis of core-shell nanoparticles and uses of said nanoparticles for surface-enhanced raman spectroscopy |
| CN109202064A (en) * | 2018-10-31 | 2019-01-15 | 大连民族大学 | A kind of short-cut method characterizing gold nanocrystals lattice structure and purity |
| CN110753838A (en) * | 2017-05-10 | 2020-02-04 | 苏黎世联邦理工学院 | Method, use and apparatus for surface enhanced Raman spectroscopy |
| CN110773748A (en) * | 2019-10-29 | 2020-02-11 | 清华大学 | Silver shell stripping method and system for gold-silver core-shell nanospheres based on femtosecond laser |
| CN112692298A (en) * | 2020-12-01 | 2021-04-23 | 中国人民解放军战略支援部队航天工程大学 | Preparation method of core-shell structure nano gold and silver composite material substrate |
| CN113433110A (en) * | 2021-06-22 | 2021-09-24 | 西安邮电大学 | Preparation method for generating substrate with honeysuckle dendritic crystal flower-like nano structure by in-situ substitution method |
-
2021
- 2021-10-08 CN CN202111171041.3A patent/CN114226743B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102251286A (en) * | 2011-07-08 | 2011-11-23 | 中国科学院理化技术研究所 | Micron/nano cone array of germanium and preparation method thereof |
| CN103526291A (en) * | 2013-10-28 | 2014-01-22 | 中国工程物理研究院化工材料研究所 | Surface enhanced Raman scattering substrate, preparation method therefor and application thereof |
| CN104155284A (en) * | 2014-08-15 | 2014-11-19 | 中国工程物理研究院化工材料研究所 | ZnO-Ag surface enhanced Raman scattering chip, and making method, preserving method and use thereof |
| CN104404624A (en) * | 2014-11-28 | 2015-03-11 | 中国科学院合肥物质科学研究院 | Controllable preparation method of three-dimensional nano plasmon polariton super crystals |
| WO2018069646A1 (en) * | 2016-10-13 | 2018-04-19 | Universite Paris Diderot | Synthesis of core-shell nanoparticles and uses of said nanoparticles for surface-enhanced raman spectroscopy |
| CN107101989A (en) * | 2017-03-16 | 2017-08-29 | 安徽中科赛飞尔科技有限公司 | Construction method based on Parameter adjustable control self-assembled structures substrate and its SERS detection methods for drugs |
| CN110753838A (en) * | 2017-05-10 | 2020-02-04 | 苏黎世联邦理工学院 | Method, use and apparatus for surface enhanced Raman spectroscopy |
| CN109202064A (en) * | 2018-10-31 | 2019-01-15 | 大连民族大学 | A kind of short-cut method characterizing gold nanocrystals lattice structure and purity |
| CN110773748A (en) * | 2019-10-29 | 2020-02-11 | 清华大学 | Silver shell stripping method and system for gold-silver core-shell nanospheres based on femtosecond laser |
| CN112692298A (en) * | 2020-12-01 | 2021-04-23 | 中国人民解放军战略支援部队航天工程大学 | Preparation method of core-shell structure nano gold and silver composite material substrate |
| CN113433110A (en) * | 2021-06-22 | 2021-09-24 | 西安邮电大学 | Preparation method for generating substrate with honeysuckle dendritic crystal flower-like nano structure by in-situ substitution method |
Non-Patent Citations (4)
| Title |
|---|
| Nanoscale flexible Ag grating/AuNPs self-assembly hybrid for ultra-sensitive sensors;Dong, J等;《NANOTECHNOLOGY》;第32卷(第15期) * |
| Nanoscale Vertical Arrays of Gold Nanorods by Self-Assembly: Physical Mechanism and Application;Jun Dong等;《 Nanoscale Research Letters》(第118期) * |
| 孙守田.《化验员基本知识》.石油化学工业出版社,1977,第165页. * |
| 金银纳米颗粒的阵列组装制备及其表面增强拉曼和表面催化反应研究;卢珠;《中国优秀硕士学位论文全文数据库 工程科技I辑》;B014-1283页 * |
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