CN108417475A - A kind of preparation method of the metal Nano structure array based on interface induced growth - Google Patents
A kind of preparation method of the metal Nano structure array based on interface induced growth Download PDFInfo
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- CN108417475A CN108417475A CN201810080098.4A CN201810080098A CN108417475A CN 108417475 A CN108417475 A CN 108417475A CN 201810080098 A CN201810080098 A CN 201810080098A CN 108417475 A CN108417475 A CN 108417475A
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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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- 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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- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
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- 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 present invention relates to a kind of preparation methods of the metal Nano structure array based on interface induced growth, include the following steps：One, substrate cleans；Two, template shifts, and ultra-thin porous alumina formwork is transferred on the substrate cleaned up；Three, adhesion strength is adjusted, and the sample that step 2 is obtained stands a few hours, keeps the adhesion strength between template and substrate partially relaxed, or reinforces the adhesion strength of template and substrate by process annealing；Four, metal deposit, using physical gas-phase deposite method in the sample surfaces deposited metal obtained by step 3；Five, template is removed, and after the completion of deposition, is removed template using adhesive tape, i.e., is left orderly metal Nano structure array in substrate surface：The situation of adhesion strength relaxation will obtain ordered nano hole array, and the situation that adhesion strength is reinforced will obtain ordered nano ring array.The method of the present invention simple process and low cost is honest and clean, extends to wafer scale.
Description
Technical field
The present invention relates to the preparation method of metal Nano structure array, more particularly, to a kind of based on interface induced growth
The preparation method of metal Nano structure array, belongs to technical field of nanometer material preparation.
Background technology
Surface phasmon is collective oscillation of the metallic surfaces conduct electronics under incident light electric field excitation so that metal
Nanostructure shows some peculiar optical properties, causes the common concern of people, in opto-electronic conversion, imaging display
The numerous areas such as part, biochemistry sensing have huge application prospect.By control the shape of metal Nano structure, size,
The type of dielectric environment and array, period, spacing etc. can effectively adjust its surface phasmon optical characteristics
Control, to meet specific application demand.Using micro-nano technology technology, such as electron beam lithography, focused ion beam grinding, phase shift light
The technologies such as quarter can prepare the metal Nano structure of various different-shapes, and accurately be controlled to nanostructure and its array
System, but this kind of technology usually requires expensive equipment and takes, it is difficult to realize that large area is prepared and applied.Chemical method can be made
Standby variously-shaped and size metal nanoparticle, but be difficult to form orderly array, and the surface-active in building-up process
Agent can be such that the optic response of metal complicates.The self assembly of association colloid ball and reactive ion etching, the method for metal deposit, pass through
It is self-assembly of the orderly two-dimensional array of colloidal spheres, then utilizes reactive ion etching to reduce the size of colloidal spheres, then pass through heat
The technologies such as evaporation, sputtering can obtain orderly metal nanoparticle and nanometer by metal deposit to the gap of colloid ball array
Hole array.But due to the inevitable defect of colloid two dimensional crystal so that this method is still deposited in terms of large area homogeneity
In problem.Therefore, there is an urgent need to the technologies of preparing of Development of Novel, effective metal Nano structure array.
The pattern of metal Nano structure is determined by its nucleation, in physical vapour deposition (PVD), gold
Category is randomly nucleated in substrate surface, forms unordered metal nanoparticle array, and further deposition will lead to these nanometers
Particle merges and finally obtains metallic film.According to heterogeneous nucleation theory, metal needs will overcome a nucleation energy barrier that could be formed
Stable core, and the introducing of template will change metal substrate surface nucleation properties.The present invention is based on such skill
What art background proposed.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of the metal Nano structure array based on interface induced growth.
The present invention utilizes ordered porous alumina template, it is proposed that a kind of to be obtained orderly by interface induced nucleation and growth
The method of metal nano ring and nanohole array.This method simple process and low cost is honest and clean, and the metal Nano structure array of preparation can
Control property is good, it is easy to accomplish prepared by large area.
The present invention proposes a kind of method preparing orderly metal Nano structure array, and steps are as follows for the method：
（1）Substrate cleans, and the substrates such as silicon chip or quartz plate is immersed in the mixed solution of the concentrated sulfuric acid and hydrogen peroxide and is heated to 90 DEG C,
It washes down 60 minutes, then after being cleaned by ultrasonic 15 minutes in acetone, ethyl alcohol, deionized water respectively, is dried up with nitrogen；
（2）Template shifts, and the PMMA ultra-thin porous alumina formworks supported is placed in the substrate surface cleaned up, then in acetone
PMMA layers are removed in solution, and ultrathin alumina template is transferred on substrate；
（3）Adhesion strength is adjusted, and substrate of the surface with alumina formwork is stood a few hours so that adherency between template and substrate
Power is partially relaxed, or reinforces the adhesion strength of template and substrate by process annealing；
（4）Substrate of the surface with alumina formwork is transferred in deposit cavity by metal deposit, and template is used towards source metal
Physical gas-phase deposite method deposited metal；
（5）Template is removed, and after the completion of deposition, removes template using adhesive tape, orderly metal nano-void battle array is left in substrate surface
Row or nano-rings array depend on the adhesion strength between template and substrate.
In the preparation method of above-mentioned metal Nano structure array, the thickness of alumina formwork is not more than 1 in the step 2
Micron.
In the preparation method of above-mentioned metal Nano structure array, step 3 process annealing passes through heating plate or annealing
Stove carries out, and annealing temperature is 150-250 DEG C, and the time is 2-5 hours.
In the preparation method of above-mentioned metal Nano structure array, physical gas-phase deposite method includes heat in the step 4
Evaporation, electron beam evaporation and magnetron sputtering, source metal include gold, silver, aluminium, copper etc., and deposition rate is 0.1-0.3 nm/s, deposition
Thickness is depending on required structure size.
In the preparation method of above-mentioned metal Nano structure array, the situation of adhesion strength relaxation will obtain in the step 5
Ordered nano hole array, the situation that adhesion strength is reinforced will obtain ordered nano ring array.
According to nucleation theory, the size of metal is formed on foreign substrate surface in physical vapour deposition (PVD) stabilization nucleus and
Nucleation energy is determined by the body free energy of nucleus and the balance of surface free energy.The major obstacle of nucleation is that occur when generating nucleus
Gas-solid interface needs to provide interface energy thus.If nucleus depends on existing interface and is formed, the gas-solid interface of high-energy
It can just can be replaced by the interface between the nucleus of low energy and nucleation matrix, it is clear that generation institute of this interface replacement than interface
The energy needed wants much less.Therefore, the presence at interface can substantially reduce nucleation energy barrier, those can make system free energy minimization
Interface will be preferential nucleating point.For simple substrate surface, the interface between template and substrate provides more
Low nucleation energy barrier.In the present invention, the adhesion strength between porous alumina formwork and substrate is weaker, when interface adhesion strength by into
One step relaxation, metallic atom are then diffused easily into up to interface area and are preferentially nucleated herein, subsequent nuclei growth, merging, are formed
Continuous network, nanohole array can be obtained by further growing.The period of array and the cycle phase of template are same, and nano-pore
Diameter determined by the amount of deposited metal.When reinforcing the adhesion strength between template and substrate by annealing, metallic atom is then not easy
It is nucleated at the step for being diffused into interface area, but being formed between template and substrate, i.e., is nucleated in bore edges, then grows up, close
And and gradually to hole central growth, form nano-rings.The outer diameter of nano-rings is determined that the internal diameter of ring is by depositing by the aperture of template
The amount of metal determines.This method simple process and low cost is honest and clean, extends to wafer scale.
Description of the drawings
Attached drawing 1 is the step schematic diagram of the method for the invention；
Attached drawing 2 is the stereoscan photograph for the silver nanoparticle hole array that embodiment 1 is prepared；
Attached drawing 3 is the stereoscan photograph for the silver nanoparticle ring array that embodiment 2 is prepared.
Specific implementation mode
The specific steps of 1 the present invention will be described in detail the method referring to the drawings.
Embodiment 1：
（1）Silicon chip is impregnated 1 hour in 90 DEG C of the concentrated sulfuric acid and the mixed solution of hydrogen peroxide, then respectively propyl alcohol, ethyl alcohol,
It is cleaned by ultrasonic 15 minutes or more in deionized water, then is rinsed well with a large amount of deionized water, is finally dried up with nitrogen.
（2）Water is dripped in the silicon chip surface cleaned up, by polymethyl methacrylate（PMMA）What is supported is ultra-thin more
Porous aluminum oxide template is adhered to silicon face surface.Then sample is placed in propanol solution and is impregnated 5-10 minutes, remove PMMA layers, it will
Template is transferred on silicon substrate, then is cleaned once with clean propanol solution, is dried.
（3）Adhesion strength between porous alumina formwork and substrate is weaker, and sample is stood a few hours, makes template and substrate
Between the further relaxation of adhesion strength.
（4）Substrate of the surface with alumina formwork is transferred in deposit cavity, template is towards evaporation source, using thermal evaporation
Method deposition of silver, deposition rate are 0.2 nm/s, and deposition thickness is 100 nm.Since the adhesion strength between template and substrate is speeded
Henan, silver atoms diffuse easily into interface area, and are preferentially nucleated in interface area, and nanometer is gradually grown between template and substrate
Hole array.
（5）After the completion of deposition, template is removed using adhesive tape, i.e., leaves silver nanoparticle hole array in substrate surface.
Embodiment 2：
（1）Silicon chip is impregnated 1 hour in 90 DEG C of the concentrated sulfuric acid and the mixed solution of hydrogen peroxide, then respectively propyl alcohol, ethyl alcohol,
It is cleaned by ultrasonic 15 minutes or more in deionized water, then is rinsed well with a large amount of deionized water, is finally dried up with nitrogen.
（2）Water is dripped in the silicon chip surface cleaned up, the PMMA ultra-thin porous alumina formworks supported are adhered to
Silicon face surface.Then sample is placed in propanol solution and is impregnated 5-10 minutes, removed PMMA layers, template is transferred to silicon substrate
On, then cleaned once with clean propanol solution, it dries.
（3）Adhesion strength between porous alumina formwork and substrate is weaker, reinforces template and silicon substrate by process annealing
Between adhesion strength, process annealing carried out by heating plate, and annealing temperature is 150 DEG C, and the time is 4 hours.
（4）Substrate of the surface with alumina formwork is transferred in deposit cavity, template is towards evaporation source, using thermal evaporation
Method deposition of silver, deposition rate are 0.2 nm/s, and deposition thickness is 50 nm.Since the adhesion strength between template and substrate is reinforced,
Silver atoms are not easy to be diffused into interface area, but are preferentially nucleated in the stepped region that template and substrate are formed, and gradually to hole center
Domain is grown, and forms nano-rings.
（5）After the completion of deposition, template is removed using adhesive tape, silver nanoparticle ring array is left in substrate surface.
Embodiment 3：
（1）Silicon chip is impregnated 1 hour in 90 DEG C of the concentrated sulfuric acid and the mixed solution of hydrogen peroxide, then respectively propyl alcohol, ethyl alcohol,
It is cleaned by ultrasonic 15 minutes or more in deionized water, then is rinsed well with a large amount of deionized water, is finally dried up with nitrogen.
（2）Water is dripped in the silicon chip surface cleaned up, the PMMA ultra-thin porous alumina formworks supported are adhered to
Silicon face surface.Then sample is placed in propanol solution and is impregnated 5-10 minutes, removed PMMA layers, template is transferred to silicon substrate
On, then cleaned once with clean propanol solution, it dries.
（3）Adhesion strength between porous alumina formwork and substrate is weaker, and sample is stood a few hours, makes template and substrate
Between the further relaxation of adhesion strength.
（4）Substrate of the surface with alumina formwork is transferred in deposit cavity, template is towards evaporation source, using thermal evaporation
Method deposition gold, deposition rate are 0.2 nm/s, and deposition thickness is 100 nm.Since the adhesion strength between template and substrate is speeded
Henan, gold atom diffuses easily into interface area, and is preferentially nucleated in interface area, and nanometer is gradually grown between template and substrate
Hole array.
（5）After the completion of deposition, template is removed using adhesive tape, gold nano hole array is left in substrate surface.
Embodiment 4：
（1）Silicon chip is impregnated 1 hour in 90 DEG C of the concentrated sulfuric acid and the mixed solution of hydrogen peroxide, then respectively propyl alcohol, ethyl alcohol,
It is cleaned by ultrasonic 15 minutes or more in deionized water, then is rinsed well with a large amount of deionized water, is finally dried up with nitrogen.
（2）Water is dripped in the silicon chip surface cleaned up, the PMMA ultra-thin porous alumina formworks supported are adhered to
Silicon face surface.Then sample is placed in propanol solution and is impregnated 5-10 minutes, removed PMMA layers, template is transferred to silicon substrate
On, then cleaned once with clean propanol solution, it dries.
（3）Adhesion strength between porous alumina formwork and substrate is weaker, reinforces template and silicon substrate by process annealing
Between adhesion strength, process annealing carried out by heating plate, and annealing temperature is 150 DEG C, and the time is 4 hours.
（4）Substrate of the surface with alumina formwork is transferred in deposit cavity, template is towards evaporation source, using thermal evaporation
Method deposition gold, deposition rate are 0.2 nm/s, and deposition thickness is 50 nm.Since the adhesion strength between template and substrate is reinforced,
Gold atom is not easy to be diffused into interface area, but is preferentially nucleated in the stepped region that template and substrate are formed, and gradually to hole center
Domain is grown, and forms nano-rings.
（5）After the completion of deposition, template is removed using adhesive tape, Gin Nanometer globoid array is left in substrate surface.
Claims (5)
1. a kind of preparation method of the metal Nano structure array based on interface induced growth, it is characterised in that：This method utilizes
Interface induced metal nucleation carries out as follows with growth, the method：
（1）Substrate cleans, and the substrates such as silicon chip or quartz plate is immersed in the mixed solution of the concentrated sulfuric acid and hydrogen peroxide and is heated to 90 DEG C,
It washes down 60 minutes, then after being cleaned by ultrasonic 15 minutes in acetone, ethyl alcohol, deionized water respectively, is dried up with nitrogen；
（2）Template shifts, and the PMMA ultra-thin porous alumina formworks supported is placed in the substrate surface cleaned up, then in acetone
PMMA layers are removed in solution, and ultrathin alumina template is transferred on substrate；
（3）Adhesion strength is adjusted, and substrate of the surface with alumina formwork is stood a few hours so that adherency between template and substrate
Power is partially relaxed, or reinforces the adhesion strength of template and substrate by process annealing；
（4）Substrate of the surface with alumina formwork is transferred in deposit cavity by metal deposit, and template is used towards source metal
Physical gas-phase deposite method deposited metal；
（5）Template is removed, and after the completion of deposition, is removed template using adhesive tape, is then left metal nano hole array in substrate surface
Or nano-rings array, depend on the adhesion strength between template and substrate.
2. the preparation method of the metal Nano structure array according to claim 1 based on interface induced growth, feature
It is：The thickness of alumina formwork is not more than 1 micron in the step 2.
3. the preparation method of the metal Nano structure array according to claim 1 based on interface induced growth, feature
It is：Low-temperature anneal temperature is 150-250 DEG C in the step 3, and the time is 2-5 hours.
4. the preparation method of the metal Nano structure array according to claim 1 based on interface induced growth, feature
It is：Physical gas-phase deposite method includes thermal evaporation, electron beam evaporation and magnetron sputtering in the step 4, source metal include gold,
Silver, aluminium, copper etc., deposition rate are 0.1-0.3 nm/s, and deposition thickness is depending on required structure size.
5. the preparation method of the metal Nano structure array according to claim 1 based on interface induced growth, feature
It is：The situation of adhesion strength relaxation will obtain ordered nano hole array in the step 5, and the situation that adhesion strength is reinforced will be had
Sequence nano-rings array.
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Cited By (3)
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| CN110127661A (en) * | 2019-05-11 | 2019-08-16 | 复旦大学 | The method that the interface induced assembling of inorganic salts prepares sequential 2 D meso-porous nano piece |
| CN110616408A (en) * | 2019-09-18 | 2019-12-27 | 北京工业大学 | Preparation method of multilayer metal nanostructure based on two-dimensional material |
| CN112725888A (en) * | 2021-01-22 | 2021-04-30 | 东北师范大学 | Method for preparing high-quality semiconductor single crystal film by using array buffer layer |
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| CN112725888A (en) * | 2021-01-22 | 2021-04-30 | 东北师范大学 | Method for preparing high-quality semiconductor single crystal film by using array buffer layer |
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