CN103011181A - Stripping-transplanting method of silicon dioxide nanowire array - Google Patents
Stripping-transplanting method of silicon dioxide nanowire array Download PDFInfo
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- CN103011181A CN103011181A CN2012105437097A CN201210543709A CN103011181A CN 103011181 A CN103011181 A CN 103011181A CN 2012105437097 A CN2012105437097 A CN 2012105437097A CN 201210543709 A CN201210543709 A CN 201210543709A CN 103011181 A CN103011181 A CN 103011181A
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Abstract
The invention discloses a stripping-transplanting method of a silicon dioxide nanowire array, which comprises the following steps: preparing a porous silver film on a silicon wafer by a solution deposition process; by using the silver film as catalytic metal, putting the silver film into a hydrofluoric acid/oxydol solution to carry out metal catalytic chemical etching so as to prepare a silicon nanowire array structure on the silicon wafer; putting in a water solution containing ammonia water to prepare a silicon dioxide nanowire array structure with small bonding force with the silicon substrate under the catalytic oxidation and etching actions of the metal silver on the ammonia water; taking out the sample, and applying a silica gel layer; after the silica gel solidifies, taking off the silica gel layer to implement stripping of the silicon dioxide nanowire array from the silicon substrate; and bonding the organic substance film with the nanowire array with any substrate by using silver adhesive to implement the transfer of the silicon dioxide nanowire array. The method is simple to operate and low at cost, and can be used for large-scale production.
Description
Technical field
The present invention relates to a kind of manufacture craft of nanometer silica line array, relate in particular to peeling off-implantation method of a kind of nanometer silica line array.
Background technology
The nanometer silica line array causes more and more people's attention with its unique character.The nanometer silica line array has important application prospect in modified rubber, engineering plastics, biomedicine, optics, novel sensor, energy transformation and nanoelectronics.
But, since growth the silicon chip of nanometer silica line array itself is arranged is rigid material, so seriously limited its range of application, so development is simple, the peeling off of nanometer silica line array-transfer techniques is vital efficiently.There is no comparatively ideal method in the prior art and realize that the nanometer silica line array easily peels off-shift.
Summary of the invention
The purpose of this invention is to provide peeling off-implantation method of a kind of low cost, simple, efficient nanometer silica line array.
The objective of the invention is to be achieved through the following technical solutions:
Peeling off-implantation method of nanometer silica line array of the present invention comprises step:
A, silicon chip pre-treatment: clean monocrystalline silicon piece;
The preparation of porous silverskin on B, the silicon chip: the 0.085g Silver Nitrate is dissolved in the deionized water, add again the 20ml mass concentration and be 40% hydrofluoric acid, then add deionized water to 100ml, after stirring, put into the silicon chip that steps A was cleaned, under 25 ℃ of room temperatures, leave standstill deposition silverskin 2min;
The preparation of silicon nanowire array on C, the silicon chip: get the 4.1ml mass concentration and be 30% hydrogen peroxide and 20ml mass concentration and be 40% hydrofluoric acid, the adding deionized water is mixed with the etching solution of 100ml, etching solution is put into the silicon chip of porous silverskin in the surface that makes among the step B under 25 ℃ of room temperatures, leave standstill etching 10min, obtain the surface with the silicon chip of silicon nanowire array structure.
D, argent catalysis ammoniacal liquor oxidation and etching, preparation is connected the little nanometer silica line array structure of power with substrate: get mass concentration and be 25～28% ammoniacal liquor and joined in 1: 100 by volume and prepare etching liquid in the deionized water, this etching solution is put into the silicon chip of nanowire array structure in the surface for preparing among the step C, then under 60 ℃ of water bath condition, leave standstill etching 5-10min, make and be connected the very little nanometer silica line array structure of power with silicon chip;
Peeling off of E, nanometer silica line array: the sample surfaces in step D drips and is coated with one deck silica gel and leaves standstill 24h or solidify by accelerating silica gel under 25 ℃ of conditions of room temperature, after silica gel solidifies, it is peeled, obtain the surface with the silica gel thin film of nanometer silica line array;
The transfer of F, nanometer silica line array: get surface in the step e with the silica gel with the nanometer silica line array, by elargol the nano-wire array face of silica gel is adhered on the flexible sarin film.
As seen from the above technical solution provided by the invention, peeling off-implantation method of the nanometer silica line array that the embodiment of the invention provides, by using solution-deposition method, at silicon chip preparation one deck porous silverskin, with this silverskin as catalytic metal, put into hydrofluoric acid/hydrogen peroxide solution and carry out the metal catalytic chemical milling, prepare silicon nanowire array structure at silicon chip, put into again the aqueous solution that is added with ammoniacal liquor, by argent catalysis ammoniacal liquor oxidation and etching, prepare the nanometer silica line array structure that is connected power little (even desorption) with silicon substrate, apply one deck medium organism (for example silica gel) thereon after taking out sample, take this layer organic thin film after solidifying off, can realize that the nanometer silica line array peels off from silicon substrate, can the organic thin film and any substrate mutually bonding (afterwards, also can fall vehicular organic matter removal) of this layer with nano-wire array, realize the transfer of nanometer silica line array by binding agent (for example elargol).This method is simple to operate, and cost is low, can be used for scale operation.
Description of drawings
The process flow diagram of the peeling off of the nanometer silica line array that Fig. 1 provides for the embodiment of the invention-implantation method.
Embodiment
The below will be described in further detail the embodiment of the invention.
Peeling off-implantation method of nanometer silica line array of the present invention, its better embodiment is:
Comprise step:
A, silicon chip pre-treatment: clean monocrystalline silicon piece;
The preparation of porous silverskin on B, the silicon chip: the 0.085g Silver Nitrate is dissolved in the deionized water, add again the 20ml mass concentration and be 40% hydrofluoric acid, then add deionized water to 100ml, after stirring, put into the silicon chip that steps A was cleaned, under 25 ℃ of room temperatures, leave standstill deposition silverskin 2min;
The preparation of silicon nanowire array on C, the silicon chip: get the 4.1ml mass concentration and be 30% hydrogen peroxide and 20ml mass concentration and be 40% hydrofluoric acid, the adding deionized water is mixed with the etching solution of 100ml, etching solution is put into the silicon chip of porous silverskin in the surface that makes among the step B under 25 ℃ of room temperatures, leave standstill etching 10min, obtain the surface with the silicon chip of silicon nanowire array structure.
D, argent catalysis ammoniacal liquor oxidation and etching, preparation is connected the little nanometer silica line array structure of power with substrate: get mass concentration and be 25～28% ammoniacal liquor and joined in 1: 100 by volume and prepare etching liquid in the deionized water, this etching solution is put into the silicon chip of nanowire array structure in the surface for preparing among the step C, then under 60 ℃ of water bath condition, leave standstill etching 5-10min, make and be connected the very little nanometer silica line array structure of power with silicon chip;
Peeling off of E, nanometer silica line array: the sample surfaces in step D drips and is coated with one deck silica gel and leaves standstill 24h or solidify by accelerating silica gel under 25 ℃ of conditions of room temperature, after silica gel solidifies, it is peeled, obtain the surface with the silica gel thin film of nanometer silica line array;
The transfer of F, nanometer silica line array: get surface in the step e with the silica gel with the nanometer silica line array, by elargol the nano-wire array face of silica gel is adhered on the flexible sarin film.
Among the described step C, control the length of nano wire by the control etching period.
In the described step e,,, then remove with nitric acid if do not need this layer silverskin with the porous silverskin with the top of the nano wire on the silica gel thin film of nanometer silica line array on the surface that makes.
Described steps A comprises:
Use first acetone ultrasonic cleaning monocrystalline silicon piece, be the ammoniacal liquor of 25%-28% again with mass concentration: mass concentration is 30% hydrogen peroxide: the mixed solution ultrasonic cleaning monocrystalline silicon piece of deionized water=1: 1: 5 volume ratio, use again deionized water ultrasonic cleaning monocrystalline silicon piece.
The present invention uses solution-deposition method, at silicon chip preparation one deck porous silverskin, with this silverskin as catalytic metal, put into hydrofluoric acid/hydrogen peroxide solution and carry out the metal catalytic chemical milling, prepare silicon nanowire array structure at silicon chip, put into again the aqueous solution that is added with ammoniacal liquor, by argent catalysis ammoniacal liquor oxidation and etching, prepare the nanometer silica line array structure that is connected power little (even desorption) with silicon substrate, apply one deck medium organism (for example silica gel) thereon after taking out sample, take this layer organic thin film after solidifying off, can realize that the nanometer silica line array peels off from silicon substrate, can be mutually bonding (afterwards with any substrate with the organic thin film of nano-wire array this layer by binding agent (for example elargol), also can fall vehicular organic matter removal), realize the transfer of nanometer silica line array.This method is simple to operate, and cost is low, can be used for scale operation.
Argent catalysis ammoniacal liquor oxidation-etching method of the present invention is so that be connected power very little (even desorption) between nanometer silica line array and silicon substrate, can very easily realize peeling off and shifting of Large-Area-Uniform nano-wire array by means of organic binder bond, and target substrate substantially unrestricted (flexible or inflexibility).
Of the present inventionly prepare easily the nanometer silica line array structure of peeling off-shifting based on argent catalysis ammoniacal liquor oxidation-etching method, low-cost, simple, efficient, after the ammoniacal liquor etch processes, original silicon nanowires be oxidized to silicon-dioxide and with silicon chip between be connected power and also become very a little less than, can be easy to strip down.Present method only need to be prepared suitable ammoniacal liquor etchant concentration and suitable bath temperature, just can make the nanometer silica line array structure of easily peeling off-shifting of Large-Area-Uniform.
The method that the present invention prepares easily the nanometer silica line array structure of peeling off-shifting is: by at Silver Nitrate (AgNO
3)/hydrofluoric acid (HF) aqueous solution deposition for some time, at silicon chip preparation one deck porous silverskin, as the etching catalytic metal, put into hydrofluoric acid (HF)/hydrogen peroxide (H with this silverskin
2O
2) carry out etching in the solution, prepare silicon nanowire array structure.In etched process, the porous silverskin is in the root of nano wire all the time in the process that moves downward.Then sample is put into ammoniacal liquor (NH
4OH) in the solution, be incubated for some time in the high temperature bath, silicon nanowires is oxidized to nanometer silica line, the nano wire root is under the catalytic etching of silverskin simultaneously, at first attenuate even break away from silicon substrate, to be connected power very weak with substrate silicon thereby prepare, the nanometer silica line array structure of easily peeling off, and the porous silverskin still sticks in the root of nano wire, by applying one deck medium organism at silicon chip surface (as silica gel, poly-fluoro-resin etc.), after organism solidifies, peel, can realize the nanometer silica line array structure peel off (this moment former silicon nanowire array structure root become the top of present nanometer silica line array structure, and covered the netted silverskin of one deck).Use binding agent, can be easily got on (afterwards, also can be when peeling off used medium organic matter removal) with the substrate of wanting that the organic film of nanowire array structure shifts in the surface, realize the transfer of silicon nanowire array structure.
The characteristics of this method have following some:
The nanometer silica line array structure is made by the silicon nanowire array structure oxidation.
Silicon nanowire array through argent catalysis ammoniacal liquor oxidation-etch processes after, the nano wire root becomes very thin even breaks away from silicon substrate, this so that between nanowire array structure and bottom silicon chip to be connected power very little, be easy to realize peeling off of nano-wire array.
Nanometer silica line top after peeling off (former silicon nanowires root) is with one deck porous silverskin.
The target substrate that shifts is wide, can transfer on most solid substrate (flexible or inflexibility).
Select extensively (with rear removable or stable chemical nature) as the organism of peeling off medium.
The length of nano wire can be carried out accuracy controlling by the etched time in hydrofluoric acid/hydrogen peroxide solution.
The restriction of the not restricted standby area of this method, and very even.
Monocrystalline silicon piece can be reused.
Cost is low, and is simple to operation.
The present invention utilizes the porous silverskin for preparing on the cleaning silicon wafer as catalytic metal, prepare silicon nanowire array by etching in hydrofluoric acid/hydrogen peroxide, put into again ammonia soln, pass through argent catalysis ammoniacal liquor oxidation and etching under the high temperature bath, prepare and be connected the very little nanometer silica line array structure of power with silicon substrate, recycling organism medium and binding agent are realized peeling off-shifting of nano-wire array.
Specific embodiment:
Equipment used: ultrasonic apparatus, constant temperature water tank.
Experimental procedure, as shown in Figure 1:
The 5(volume ratio) and deionized water ultrasonic cleaning monocrystalline silicon piece 1, silicon chip pre-treatment: use successively acetone, ammoniacal liquor (mass concentration 25%-28%): hydrogen peroxide (mass concentration 30%): deionized water=1: 1:.
2, the preparation of porous silverskin on the silicon chip: 0.5mmol(0.085g) Silver Nitrate (AgNO
3) be dissolved in a certain amount of deionized water, add again 0.46mol(20ml) hydrofluoric acid (HF, mass concentration is 40%), then add deionized water to 100ml, after stirring, put into the silicon chip that step 1 was cleaned, leave standstill 25 ℃ of deposition silverskin 2min(room temperatures).
3, the preparation of silicon nanowire array on the silicon chip: prepare according to a certain ratio etching solution, get 40mmol(4.1ml) hydrogen peroxide (H
2O
2, mass concentration is 30%) and 0.46mol(20ml) hydrofluoric acid (HF, mass concentration is 40%), add the etching solution that deionized water is mixed with 100ml.Etching solution is put into the silicon chip of porous silverskin in surface in the step 2 leave standstill etching 10min(etching period difference, nanowire length is different, but accuracy controlling) (25 ℃ of room temperatures), obtain the surface with the silicon chip of silicon nanowire array structure.
4, the oxidation of argent catalysis ammoniacal liquor and etching, preparation is connected the little nanometer silica line array structure of power with substrate: ammoniacal liquor (NH is put into the silicon chip of nanowire array structure in the surface of preparation in the step 3
4HO) (mass concentration is 25～28%): deionized water=1: the 100(volume ratio) in the etching solution, then put at once constant temperature water tank, leave standstill etching 5-10min under 60 ℃ of conditions, just can make and be connected the very little nanometer silica line array structure of power with substrate.
5, peeling off of nanometer silica line array: the sample surfaces in step 4 drips to be coated with and leaves standstill 24h(under 25 ℃ of conditions of one deck silica gel (silica gel viscosity is adjustable) room temperature and also can solidify by accelerating silica gel), after silica gel solidifies, it is peeled, just can obtain the surface with the silica gel thin film of nanometer silica line array, and nano wire top (former silicon nanowires root) with the porous silverskin (certainly, if do not need this layer silverskin, also available nitric acid is removed).
6, the transfer of nanometer silica line array: get surface in the step 5 with the silica gel with the nanometer silica line array, by elargol the nano-wire array face of silica gel is adhered on the flexible sarin film.
The effect of specific embodiment:
Scanning electronic microscope (as shown in Figure 1) analytical proof peeling off-migration process of nanometer silica line array.
Among Fig. 1, the porous silverskin that (a) deposits on the silicon chip, illustration are the sectional elevation of silverskin; (b) silicon nanowire array structure (sectional elevation); (c) be connected the power nanometer silica line array structure (45° angle oblique drawing) of very little (even disengaging) with substrate, illustration is sectional elevation; (d) peel off-be transferred to the nanometer silica line array structure (45° angle oblique drawing) on the silica gel; (e) being transferred to nanometer silica line array structure (sectional elevation) on the sarin film by elargol, is layer of silica gel-nanometer silica line array layer-elargol layer-sarin rete from top to bottom successively among the figure.
The above; only for the better embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (4)
1. peeling off-implantation method of a nanometer silica line array is characterized in that, comprises step:
A, silicon chip pre-treatment: clean monocrystalline silicon piece;
The preparation of porous silverskin on B, the silicon chip: the 0.085g Silver Nitrate is dissolved in the deionized water, add again the 20ml mass concentration and be in 40% the hydrofluoric acid, then add deionized water to 100ml, after stirring, put into the silicon chip that steps A was cleaned, under 25 ℃ of room temperatures, leave standstill deposition silverskin 2min;
The preparation of silicon nanowire array on C, the silicon chip: get the 4.1ml mass concentration and be 30% hydrogen peroxide and 20ml mass concentration and be 40% hydrofluoric acid, the adding deionized water is mixed with the etching solution of 100ml, etching solution is put into the silicon chip of porous silverskin in the surface that makes among the step B under 25 ℃ of room temperatures, leave standstill etching 10min, obtain the surface with the silicon chip of silicon nanowire array structure.
D, argent catalysis ammoniacal liquor oxidation and etching, preparation is connected the little nanometer silica line array structure of power with substrate: get mass concentration and be 25～28% ammoniacal liquor and joined in 1: 100 by volume and prepare etching liquid in the deionized water, this etching solution is put into the silicon chip of nanowire array structure in the surface for preparing among the step C, then under 60 ℃ of water bath condition, leave standstill etching 5-10min, make and be connected the very little nanometer silica line array structure of power with silicon chip;
Peeling off of E, nanometer silica line array: the sample surfaces in step D drips and is coated with one deck silica gel and leaves standstill 24h or solidify by accelerating silica gel under 25 ℃ of conditions of room temperature, after silica gel solidifies, it is peeled, obtain the surface with the silica gel thin film of nanometer silica line array;
The transfer of F, nanometer silica line array: get surface in the step e with the silica gel with the nanometer silica line array, by elargol the nano-wire array face of silica gel is adhered on the flexible sarin film.
2. peeling off-implantation method of nanometer silica line array according to claim 1 is characterized in that, among the described step C, controls the length of nano wire by the control etching period.
3. nanometer silica line array according to claim 1 peels off-implantation method, it is characterized in that, in the described step e, the surface that makes with the top of the nano wire on the silica gel thin film of nanometer silica line array with the porous silverskin, if do not need this layer silverskin, then remove with nitric acid.
4. according to claim 1, the peeling off-implantation method of 2 or 3 described nanometer silica line arrays, it is characterized in that described steps A comprises:
Use first acetone ultrasonic cleaning monocrystalline silicon piece, be the ammoniacal liquor of 25%-28% again with mass concentration: mass concentration is 30% hydrogen peroxide: the mixed solution ultrasonic cleaning monocrystalline silicon piece of deionized water=1: 1: 5 volume ratio, use again deionized water ultrasonic cleaning monocrystalline silicon piece.
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| CN103337449A (en) * | 2013-04-28 | 2013-10-02 | 中国科学院合肥物质科学研究院 | Method for transplanting silicon nanowire array and preparing simple device thereof |
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| CN103521226B (en) * | 2013-11-05 | 2015-05-20 | 华东理工大学 | Catalyst with copper nanoparticles loaded on silicon nanowire array, preparing method thereof and application thereof |
| CN104045054A (en) * | 2014-05-14 | 2014-09-17 | 中国科学院合肥物质科学研究院 | Method for preparing high-adhesion micro-nano array structure film through wet etching and reverse transfer printing |
| CN104835719A (en) * | 2015-04-01 | 2015-08-12 | 浙江大学 | Porous SiO2 nanowire array preparation method |
| CN109324088A (en) * | 2017-07-31 | 2019-02-12 | 天津大学 | The heterogeneous multilevel structure of silicon nanowires and its preparation method and application of netted tungsten oxide nano modification |
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