CN108417475B - Preparation method of metal nanostructure array based on interface induced growth - Google Patents
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02587—Structure
- H01L21/0259—Microstructure
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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Abstract
The invention relates to a preparation method of a metal nano-structure array based on interface induction growth, which comprises the following steps: firstly, cleaning a substrate; secondly, template transfer, namely transferring the ultrathin porous alumina template to a cleaned substrate; thirdly, adjusting the adhesion, namely standing the sample obtained in the second step for several hours to partially relax the adhesion between the template and the substrate, or enhancing the adhesion between the template and the substrate through low-temperature annealing; depositing metal, namely depositing metal on the surface of the sample obtained in the step three by adopting a physical vapor deposition method; and fifthly, stripping the template, and stripping the template by using an adhesive tape after deposition is finished, namely, an ordered metal nano structure array is left on the surface of the substrate: the case of relaxation of the adhesion will result in an ordered nanopore array, and the case of enhanced adhesion will result in an ordered nanoring array. The method has simple process and low cost, and can be expanded to the wafer scale.
Description
Technical Field
The invention relates to a preparation method of a metal nano-structure array, in particular to a preparation method of a metal nano-structure array based on interface induced growth, and belongs to the technical field of nano-material preparation.
Background
The surface plasmon is collective oscillation of metal surface conduction electrons under the excitation of an incident electromagnetic field, so that the metal nano structure shows some peculiar optical properties, attracts general attention of people, and has great application prospect in various fields such as photoelectric conversion, imaging display devices, biochemical sensing and the like. The surface plasmon optical characteristics of the metal nano structure can be effectively regulated and controlled by controlling the shape, size, dielectric environment, array type, period, spacing and the like of the metal nano structure, so that specific application requirements are met. The metal nano structures with different morphologies can be prepared by adopting a micro-nano processing technology, such as electron beam lithography, focused ion beam grinding, phase shift lithography and the like, and the nano structures and the arrays thereof are accurately controlled, but the technology generally needs expensive equipment and consumes time, and large-area preparation and application are difficult to realize. Chemical methods can produce metal nanoparticles of various shapes and sizes, but it is difficult to form ordered arrays, and surfactants in the synthesis process complicate the optical response of the metal. The method combines the colloid ball self-assembly, the reactive ion etching and the metal deposition, forms the colloid ball ordered two-dimensional array through the self-assembly, then utilizes the reactive ion etching to reduce the size of the colloid ball, and deposits the metal into the gaps of the colloid ball array through the technologies of thermal evaporation, sputtering and the like, so as to obtain the ordered metal nano-particles and the nano-pore array. However, this method still has a problem in terms of large-area uniformity due to the inevitable defects of colloidal two-dimensional crystals. Therefore, there is an urgent need to develop new and effective techniques for preparing metal nanostructure arrays.
The morphology of the metallic nanostructures is largely determined by its nucleation, in physical vapor deposition, the metal nucleates randomly at the substrate surface, forming an array of disordered metallic nanoparticles, and further deposition will cause these nanoparticles to coalesce and ultimately result in a metallic film. According to the heterogeneous nucleation theory, the metal needs to overcome a nucleation energy barrier to form stable nuclei, and the introduction of the template changes the nucleation characteristics of the metal on the substrate surface. The present invention has been made in view of such a background.
Disclosure of Invention
The invention aims to provide a preparation method of a metal nanostructure array based on interface induced growth.
The invention provides a method for obtaining ordered metal nano-rings and nano-pore arrays by utilizing an ordered porous alumina template through interface induced nucleation and growth. The method has the advantages of simple process, low cost, good controllability of the prepared metal nanostructure array and easy realization of large-area preparation.
The invention provides a method for preparing an ordered metal nano-structure array, which comprises the following steps:
(1) cleaning a substrate, namely soaking the substrate such as a silicon wafer or a quartz wafer into a mixed solution of concentrated sulfuric acid and hydrogen peroxide, heating to 90 ℃, cleaning for 60 minutes, ultrasonically cleaning in acetone, ethanol and deionized water for 15 minutes, and drying by using nitrogen;
(2) transferring the template, namely placing the ultrathin porous alumina template supported by PMMA on the surface of a cleaned substrate, removing the PMMA layer in an acetone solution, and transferring the ultrathin alumina template to the substrate;
(3) adjusting the adhesion, namely standing the substrate with the alumina template on the surface for several hours to partially relax the adhesion between the template and the substrate, or enhancing the adhesion between the template and the substrate through low-temperature annealing;
(4) metal deposition, namely transferring the substrate with the alumina template on the surface into a deposition cavity, wherein the template faces to a metal source, and depositing metal by adopting a physical vapor deposition method;
(5) and (3) stripping the template, and stripping the template by using an adhesive tape after deposition is finished, so as to leave an ordered metal nano-hole array or nano-ring array on the surface of the substrate, wherein the ordered metal nano-hole array or the nano-ring array depends on the adhesive force between the template and the substrate.
In the preparation method of the metal nanostructure array, the thickness of the alumina template in the step 2 is not more than 1 micron.
In the preparation method of the metal nanostructure array, the step 3 low-temperature annealing is performed by a heating plate or an annealing furnace, the annealing temperature is 150-250 ℃, and the time is 2-5 hours.
In the preparation method of the metal nanostructure array, the physical vapor deposition method in the step 4 comprises thermal evaporation, electron beam evaporation and magnetron sputtering, the metal source comprises gold, silver, aluminum, copper and the like, the deposition rate is 0.1-0.3 nm/s, and the deposition thickness depends on the required structure size.
In the preparation method of the metal nanostructure array, the situation of relaxation of the adhesive force in the step 5 can obtain an ordered nanopore array, and the situation of enhancement of the adhesive force can obtain an ordered nanoring array.
According to nucleation theory, the size of stable nuclei formed on the surface of a foreign substrate by a metal in physical vapor deposition and the nucleation energy are determined by the balance of the bulk free energy and the surface free energy of the nuclei. The main obstacle to nucleation is the presence of a gas-solid interface during nucleation, for which interface energy needs to be provided. If the crystal nuclei form depending on the existing interface, the high-energy gas-solid interface energy is replaced by the interface energy between the low-energy crystal nuclei and the nucleation matrix, and apparently, the interface replacement requires much less energy than the generation of the interface. Thus, the presence of interfaces can greatly reduce the nucleation energy barrier, and those interfaces that minimize the free energy of the system will be preferential nucleation sites. The interface between the template and the substrate provides a lower nucleation energy barrier relative to a pure substrate surface. In the invention, the adhesion between the porous alumina template and the substrate is weaker, when the adhesion of the interface is further relaxed, metal atoms are easy to diffuse to reach the interface region and nucleate preferentially at the interface region, and then crystal nuclei grow up and merge to form a continuous network, and the nanopore array can be obtained by further growth. The period of the array is the same as the period of the template, and the diameter of the nanopore is determined by the amount of metal deposited. When the adhesion between the template and the substrate is enhanced by annealing, the metal atoms are not easy to diffuse to the interface region, but nucleate at the step formed between the template and the substrate, namely nucleate at the edge of the hole, grow, merge and gradually grow towards the center of the hole to form the nanoring. The outer diameter of the nanoring is determined by the pore size of the template and the inner diameter of the ring is determined by the amount of metal deposited. The method has simple process and low cost, and can be expanded to the wafer scale.
Drawings
FIG. 1 is a schematic representation of the steps of the process of the present invention;
FIG. 2 is a scanning electron micrograph of the silver nanopore array prepared in example 1;
FIG. 3 is a scanning electron micrograph of the silver nanoring array prepared in example 2.
Detailed Description
The specific steps of the method of the present invention are described in detail below with reference to FIG. 1.
Example 1:
(1) soaking the silicon wafer in a mixed solution of concentrated sulfuric acid and hydrogen peroxide at 90 ℃ for 1 hour, then ultrasonically cleaning the silicon wafer in propanol, ethanol and deionized water for more than 15 minutes, then washing the silicon wafer with a large amount of deionized water, and finally drying the silicon wafer by using nitrogen.
(2) Dripping a drop of water on the surface of the cleaned silicon wafer, and adhering the ultrathin porous alumina template supported by polymethyl methacrylate (PMMA) on the surface of the silicon surface. And then, placing the sample in a propanol solution for soaking for 5-10 minutes, removing the PMMA layer, transferring the template to a silicon substrate, cleaning once by using a clean propanol solution, and airing.
(3) The adhesion between the porous alumina template and the substrate is weak and the sample is allowed to stand for several hours to further relax the adhesion between the template and the substrate.
(4) And transferring the substrate with the alumina template on the surface into a deposition cavity, wherein the template faces to an evaporation source, and depositing silver by adopting a thermal evaporation method, wherein the deposition rate is 0.2 nm/s, and the deposition thickness is 100 nm. As the adhesion between the template and the substrate is relaxed, silver atoms readily diffuse to the interface region and nucleate preferentially at the interface region, and gradually grow into an array of nanopores between the template and the substrate.
(5) After deposition, the template is peeled off by using an adhesive tape, namely, the silver nanopore array is left on the surface of the substrate.
Example 2:
(1) soaking the silicon wafer in a mixed solution of concentrated sulfuric acid and hydrogen peroxide at 90 ℃ for 1 hour, then ultrasonically cleaning the silicon wafer in propanol, ethanol and deionized water for more than 15 minutes, then washing the silicon wafer with a large amount of deionized water, and finally drying the silicon wafer by using nitrogen.
(2) Dripping a drop of water on the surface of the cleaned silicon wafer, and adhering the ultrathin porous alumina template supported by the PMMA on the surface of the silicon surface. And then, placing the sample in a propanol solution for soaking for 5-10 minutes, removing the PMMA layer, transferring the template to a silicon substrate, cleaning once by using a clean propanol solution, and airing.
(3) The adhesion between the porous alumina template and the substrate is weak, the adhesion between the template and the silicon substrate is enhanced through low-temperature annealing, the low-temperature annealing is carried out through a heating plate, the annealing temperature is 150 ℃, and the time is 4 hours.
(4) And transferring the substrate with the alumina template on the surface into a deposition cavity, wherein the template faces to an evaporation source, and depositing silver by adopting a thermal evaporation method, wherein the deposition rate is 0.2 nm/s, and the deposition thickness is 50 nm. Because the adhesion between the template and the substrate is strengthened, silver atoms are not easy to diffuse to the interface region, but nucleate preferentially in the step region formed by the template and the substrate and gradually grow to the central region of the hole to form a nano-ring.
(5) After deposition, the template was peeled off with tape, leaving an array of silver nanorings on the substrate surface.
Example 3:
(1) soaking the silicon wafer in a mixed solution of concentrated sulfuric acid and hydrogen peroxide at 90 ℃ for 1 hour, then ultrasonically cleaning the silicon wafer in propanol, ethanol and deionized water for more than 15 minutes, then washing the silicon wafer with a large amount of deionized water, and finally drying the silicon wafer by using nitrogen.
(2) Dripping a drop of water on the surface of the cleaned silicon wafer, and adhering the ultrathin porous alumina template supported by the PMMA on the surface of the silicon surface. And then, placing the sample in a propanol solution for soaking for 5-10 minutes, removing the PMMA layer, transferring the template to a silicon substrate, cleaning once by using a clean propanol solution, and airing.
(3) The adhesion between the porous alumina template and the substrate is weak and the sample is allowed to stand for several hours to further relax the adhesion between the template and the substrate.
(4) And transferring the substrate with the alumina template on the surface into a deposition cavity, wherein the template faces to an evaporation source, and depositing gold by adopting a thermal evaporation method, wherein the deposition rate is 0.2 nm/s, and the deposition thickness is 100 nm. Since the adhesion between the template and the substrate is relaxed, gold atoms easily diffuse to the interface region and nucleate preferentially at the interface region, and gradually grow into an array of nanopores between the template and the substrate.
(5) After deposition is completed, the template is peeled off by using an adhesive tape, and a gold nanopore array is left on the surface of the substrate.
Example 4:
(1) soaking the silicon wafer in a mixed solution of concentrated sulfuric acid and hydrogen peroxide at 90 ℃ for 1 hour, then ultrasonically cleaning the silicon wafer in propanol, ethanol and deionized water for more than 15 minutes, then washing the silicon wafer with a large amount of deionized water, and finally drying the silicon wafer by using nitrogen.
(2) Dripping a drop of water on the surface of the cleaned silicon wafer, and adhering the ultrathin porous alumina template supported by the PMMA on the surface of the silicon surface. And then, placing the sample in a propanol solution for soaking for 5-10 minutes, removing the PMMA layer, transferring the template to a silicon substrate, cleaning once by using a clean propanol solution, and airing.
(3) The adhesion between the porous alumina template and the substrate is weak, the adhesion between the template and the silicon substrate is enhanced through low-temperature annealing, the low-temperature annealing is carried out through a heating plate, the annealing temperature is 150 ℃, and the time is 4 hours.
(4) And transferring the substrate with the alumina template on the surface into a deposition cavity, wherein the template faces to an evaporation source, and depositing gold by adopting a thermal evaporation method, wherein the deposition rate is 0.2 nm/s, and the deposition thickness is 50 nm. Because the adhesion between the template and the substrate is strengthened, gold atoms are not easy to diffuse to the interface region, but preferentially nucleate in the step region formed by the template and the substrate and gradually grow to the central region of the hole to form a nano-ring.
(5) After deposition is completed, the template is peeled off by using an adhesive tape, and the gold nanoring array is left on the surface of the substrate.
Claims (3)
1. A preparation method of a metal nano-structure array based on interface induction growth is characterized by comprising the following steps: the method utilizes an interface to induce metal nucleation and growth, and comprises the following steps:
(1) cleaning a substrate, namely immersing a silicon chip or quartz chip substrate into a mixed solution of concentrated sulfuric acid and hydrogen peroxide, heating to 90 ℃, cleaning for 60 minutes, ultrasonically cleaning in acetone, ethanol and deionized water for 15 minutes respectively, and drying by using nitrogen;
(2) transferring the template, namely placing the ultrathin porous alumina template supported by PMMA on the surface of a cleaned substrate, removing the PMMA layer in an acetone solution, and transferring the ultrathin alumina template to the substrate;
(3) adjusting the adhesion, namely standing the substrate with the alumina template on the surface for several hours to partially relax the adhesion between the template and the substrate, or annealing at the temperature of 150-250 ℃ to enhance the adhesion between the template and the substrate, wherein the annealing time is 2-5 hours;
(4) metal deposition, namely transferring the substrate with the alumina template on the surface into a deposition cavity, wherein the template faces to a metal source, and depositing metal by adopting a physical vapor deposition method;
(5) and (3) stripping the template, and stripping the template by using an adhesive tape after deposition is finished, so that the metal nanopore array or the nanoring array is left on the surface of the substrate, and the ordered nanopore array is obtained under the condition that the adhesive force is relaxed and the ordered nanoring array is obtained under the condition that the adhesive force is enhanced depending on the adhesive force between the template and the substrate.
2. The method for preparing the metal nanostructure array based on the interface induced growth according to claim 1, wherein: the thickness of the alumina template in the step 2 is not more than 1 micron.
3. The method for preparing the metal nanostructure array based on the interface induced growth according to claim 1, wherein: the physical vapor deposition method in the step 4 comprises thermal evaporation, electron beam evaporation and magnetron sputtering, the metal source comprises gold, silver, aluminum and copper, the deposition rate is 0.1-0.3 nm/s, and the deposition thickness is determined according to the required structure size.
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