CN101532177B - Method for preparing zinc sulfide quantum wire by using template method - Google Patents
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Abstract
The invention relates to a method for preparing a zinc sulfide quantum wire by using a template method. The method comprises that: firstly, a barrier layer and an alumina layer containing a microporous array are formed on two surfaces of an aluminum substrate in turn by using an anode oxidization method, wherein the barrier layer is an alumina layer which does not contain the microporous array, and the aperture of a micropore is 8 to 15 nanometers; secondly, the aluminum substrate is clamped in an aluminum-base removing clamp to remove the alumina layer containing the microporous array, the barrier layer and aluminum base on a central part of one surface of the aluminum substrate and the barrier layer on the back of the alumina layer on the other surface of the aluminum substrate, and the aluminum-base removing clamp is taken off to obtain an alumina nano template containing the microporous array; thirdly, a layer of gold electrodes is sputtered on the alumina layer on one surface removed with the aluminum base; and finally, the zinc sulfide quantum wire is formed in the micropore of the nano template by using a direct current deposition method. The prepared zinc sulfide quantum wire has the advantages of quite obvious quantum limit effect, huge specific surface area, high purity of the material and even density and property, and has better performance than the large-diameter zinc sulfide quantum wire prepared by background technology.
Description
Technical field
The present invention relates to a kind ofly prepare the method for zinc sulfide quantum wire with template, the technical field of metal nanometer material preparation.
Background technology
Quantum wire is meant when the diameter of material is suitable with its de broglie wavelength, the monodimension nanometer material of various quantum effects, non-localized quantum coherence effect, quantum fluctuation and chaos, photovoltaic effect and non-linear optical effect etc. can occur.Based on quantum size effect, quantum Interference, the low dimension semiconductor material of quantum tunneling effect and non-linear optical effect etc. is a kind of novel semiconductor material of manual construction, is the basis of microelectronics of new generation, opto-electronic device and circuit.Its development and application very likely trigger new technological revolution.
The quantum size effect of zinc sulfide quantum wire makes that the energy level of zinc sulphide changes, energy gap broadens, and absorbs with emmission spectrum and moves to the shortwave direction, shows as change in color on intuitively.The surface effects of quantum wire makes its specific surface area; Surface energy and Surface binding energy all increase rapidly; Cause the zinc sulfide quantum wire surface atom to transport the variation with configuration; Also cause simultaneously the variation of surface electronic spin conformation and electronic spectrum, character such as its optics, electricity and nonlinear optics are had material impact, therefore; Zinc sulfide quantum wire is huge in aspect application potential such as light, electricity, magnetic, catalysis, has attracted numerous scientific workers to carry out number of research projects in its preparation and application facet.
Metallic sulfide has excellent characteristic, and particularly zinc sulphide is a kind of II～VI family direct band-gap semicondictor, and energy gap is 3.6eV; Be widely used in dull and stereotyped device, infrared detector, photo luminescent devices, infrared window; Solar cell, transmitter, aspects such as laser apparatus and biomedicine.Chemical vapor deposition (CVD) is the effective ways of synthetic zinc sulphide monodimension nanometer material, the synthetic exigent vacuum tightness of these CVD and comparatively complex apparatus usually.In addition, study still very limited about the thing phase of zinc sulfide nano-material and the control synthetic of particle diameter at present.At present people are many to the research of zinc blende nano-wire, and its diameter is all at tens more than the nanometer, and only have the research of the zinc sulfide quantum wire about 10 nanometers quite few to diameter.With the zinc blende nano-wire of general method (such as sol-gel method, solvent-thermal method etc.) preparation, because diameter is relatively large, can not show very excellent physical characteristics, be all to exist great restriction in its application facet or on to its research.
Summary of the invention
The objective of the invention is to propose a kind of method for preparing zinc sulfide quantum wire with template.
For realizing above-mentioned purpose, the present invention adopts following technical scheme.Form blocking layer and the alumina layer that contains microwell array successively on the two sides of aluminium substrate with anode oxidation method earlier; The blocking layer is the alumina layer that does not contain microwell array; The pore size of micropore is 8～15nm; Meet quantum wire and require the size that reaches, again aluminium substrate is clamped in the blocking layer at the alumina layer back side of the alumina layer that contains microwell array on the centre portions of removing the aluminium substrate one side in the aluminium base anchor clamps, blocking layer, aluminium base and aluminium substrate another side, shed aluminium base anchor clamps; The aluminium oxide nano-form that must contain microwell array; Sputter one deck gold electrode on the alumina layer that removes aluminium base one side is last then, in the micropore of described nano-form, forms zinc sulfide quantum wire with direct current deposition method.The zinc sulfide quantum wire that makes with method of the present invention has very significantly quantum limitation effect; Specific surface area is huge, and the purity of material is high, and density and characteristic are even; Guarantee the zinc sulfide quantum wire that its diameter that makes than background technology is bigger, have excellent more performance.
Be described with reference to the accompanying drawings technical scheme of the present invention at present.
A kind ofly prepare the method for zinc sulfide quantum wire, it is characterized in that the concrete operations step with template:
The first step is cleaned substrate 4 with traditional method
Get a purity and be 99.999% aluminium flake, specification is 20mm * 20mm * 0.5mm, as substrate 4; Be placed on and carry out ultrasonic cleaning in the acetone, it is dry to put into baking oven after the cleaning, places nitrogen atmosphere again; 450 ℃～650 ℃ down annealing 4 hours～6 hours are carried out electrochemical etching then in volume ratio is 1: 4 perchloric acid and alcoholic acid mixing solutions, polish temperature is 0 ℃～10 ℃; Polishing time is 30 seconds～50 seconds, cleans substrate 4 surfaces with acid solution or alkaline solution at last;
A second step anodic oxidation
To put into the sulphuric acid soln that concentration is 12wt%～16wt% through the substrate 4 that the first step is handled; Under-6 ℃～6 ℃, carry out the anodic oxidation first time; Negative electrode and anode are respectively platinized platinum and substrate 4; Anodised voltage, electric current and time are respectively 20 volts, 1mA～10mA and 2 hours～5 hours, on the front and back of substrate 4, form straight tackling layer 3 and backside barrier layer 5 respectively, and straight tackling layer 3 is the alumina layers that do not contain microwell array with backside barrier layer 5; Then on straight tackling layer 3 and backside barrier layer 5, form front alumina layer 2 and back side alumina layer 6 respectively; Front alumina layer 2 is the alumina layers that contain microwell array with back side alumina layer 6, but the microwell array that an anodic oxidation forms, and the pore size of its micropore is even inadequately; The arrangement of its array is neat inadequately, need carry out two-step anodization;
The 3rd step two-step anodization
To put into by phosphoric acid, chromic acid and water through the substrate 4 that second step handled and mix mixing liquid; Phosphoric acid: chromic acid: the weight ratio of water is 6: 1.8: 92.2,65 ℃ of water-baths 40 minutes～60 minutes, deoxidation aluminium lamination; This alumina layer comprises front alumina layer 2, straight tackling layer 3, backside barrier layer 5 and back side alumina layer 6; Again under-6 ℃～6 ℃,, concentration carries out the anodic oxidation second time in being the sulphuric acid soln of 12wt%～15wt%, and negative electrode and anode are respectively platinized platinum and the substrate 4 handled through deoxidation aluminium film; Anodised voltage, electric current and time are respectively 20 volts, 2mA～10mA and 2 hours～5 hours; On the front and back of substrate 4, form straight tackling layer 3 and backside barrier layer 5 respectively, on straight tackling layer 3 and backside barrier layer 5, form front alumina layer 2 and back side alumina layer 6 then respectively, compare with an anodic oxidation in second step; The microwell array that two-step anodization forms; The aperture of its micropore is 8～15nm, and size is even, the marshalling of its array;
The 4th step was removed the alumina layer on substrate 4 back sides
Go aluminium base anchor clamps 7 usefulness tetrafluoroethylene to process, comprise top board 8 and base plate 11, have hole 9 in the central part office of top board 8; Hole 9 is that diameter is the circular hole of 7mm, screw 10 is respectively arranged on four jiaos of top board 8 and base plate 11, during use; Top board 8 is fixed with four screws of base plate 11 usefulness, and substrate 4 is clamped between top board 8 and the base plate 11, will be clamped in the aluminium base anchor clamps 7 through the substrate 4 that the 3rd step handled; Outside only the centre portions at substrate 4 back sides is exposed to; Again clamping substrate 4 gone aluminium base anchor clamps 7 to put into by phosphoric acid, chromic acid and water to mix mixing liquid, phosphoric acid: chromic acid: the weight ratio of water is 6: 1.8: 92.2,65 ℃ of water-baths 40 minutes～60 minutes; Remove the alumina layer on the centre portions at substrate 4 back sides, this alumina layer comprises back side alumina layer 6 and backside barrier layer 5;
The 5th step went aluminium base 40
Substrate 4 is put into the SnCl that concentration is 10wt%～16wt% with its aluminium base anchor clamps 7 that go of clamping
4In solution or the Cupric Chloride Solution, soaked 4 hours～8 hours, removing aluminium base 40, aluminium base 40 is exactly the centre portions of substrate 4;
The 6th step was removed straight tackling layer 3
Substrate 4 is put into the phosphoric acid that concentration is 6wt% with its aluminium base anchor clamps 7 that go of clamping; 30 ℃ were reacted 10 minutes～16 minutes down, removed straight tackling layer 4, unloaded down aluminium base anchor clamps 7; Obtain containing the substrate 4 of front alumina layer 2, promptly contain the alumina layer nano-form 12 of microwell array;
The 7th step sputter Au electrode
With the back spatter layer of Au electrode of the 6th aluminium oxide nano-form that contains microwell array 12 that make of step, thickness is 200 nanometers;
The 8th step obtain solution
At room temperature, preparation contains 7.5gL
-1ZnCl
2And 6.1gL
-1The dimethyl sulphoxide solution of sulphur simple substance;
The 9th step dc electrodeposition
The aluminium base anchor clamps 7 that go of the alumina layer nano-form 12 that contains microwell array that clamping was handled through the 7th step are put into the solution of the 8th step preparation, under 120 ℃, carry out dc electrodeposition, and current density is 6.62mA/cm
2The alumina layer nano-form 12 that contains microwell array that anode and negative electrode are respectively platinized platinum and handle through the 7th step deposits 10 minutes～20 minutes, in the micropore 1 of the microwell array of this nano-form, forms zinc sulfide quantum wire; Take out this nano-form; Use dimethyl sulphoxide solution, acetone and deionized water rinsing clean successively, seasoning under the room temperature makes the zinc sulfide quantum wire in the microwell array that is stored in the alumina layer nano-form 12 that contains microwell array.
Zinc sulfide quantum wire can be widely used in fields such as nano-fabrication technique, electronic technology and device, biotechnology, medicine, chemistry.Quantum device have the emission threshold value low, emission is big, the field emission performance of stable high excellence.Utilize the principle of quantum line traffic control impurity scattering, can be made into quantum wire slot field-effect transistor (FET), the single-mode quantum line can be made electron interference effect devices such as A-B quantum interference FET and bragg reflection quantum interference FET.
Compare with background technology, the present invention has the following advantages:
1, preparation method of the present invention comes to control effectively the size of zinc sulfide quantum wire through the alumina formwork of preparation small-bore; Guarantee that it has quantum effect; Then regulate energy gap by quantum limitation effect, make ZnS have the uptake factor more much bigger than body material.
2, preparation method of the present invention is simple, and cost of manufacture is low, and is pollution-free.
Description of drawings
Fig. 1: remove the top board of aluminium base anchor clamps 7 and the vertical view of base plate.Go aluminium base anchor clamps 7 usefulness tetrafluoroethylene to process, wherein, the 7th, remove aluminium base anchor clamps, the 8th, top board, 9 is circular hole, diameter is 7mm, the 10th, screw, diameter are 2.5mm, the 11st, base plate, thickness, length and the width of top board 8 and base plate 11 are respectively 8mm, 4cm and 4cm.
Fig. 2: the diagrammatic cross-section of the substrate 4 that the 3rd step of warp handles.Wherein, 1 is micropore, and its aperture is 8～15nm, and 2 is the front alumina layer, and 3 is the straight tackling layer, and 4 is substrate, and 40 is aluminium base, and 5 is backside barrier layer, and 6 is back side alumina layer.
Fig. 3: surface scan electron microscope (SEM) image of the substrate 4 that the 3rd step of warp handles.
Fig. 4: the diagrammatic cross-section that contains the alumina layer nano-form 12 of microwell array.Wherein, the 12nd, contain the alumina layer nano-form of microwell array.
Embodiment
Combine accompanying drawing and embodiment to specify technical scheme of the present invention at present.All embodiment all operate according to the operation steps of " summary of the invention " said method.Therefore, all embodiment is only enumerated the gordian technique data of each operation steps.
Embodiment 1
In the first step, substrate 4 is 450 ℃ of down annealing 4 hours, 0 ℃ of following electrochemical etching 30 seconds; In second step, the concentration of sulphuric acid soln is 12wt%, and once anodised temperature is-6 ℃, and anodizing time and electric current were respectively 2 hours and 10mA; In the 3rd step, the water-bath time is 40 minutes, and the concentration of sulphuric acid soln is 12wt%, and the temperature of two-step anodization is-6 ℃, and anodizing time and electric current were respectively 2 hours and 10mA; In the 4th step, water-bath 40 minutes; In the 5th step, removing aluminium base 40 solution is that concentration is the SnCl of 10wt%
4Solution, soak time are 8 hours; In the 6th step, the reaction times is 10 minutes; In the 9th step, depositing time is 10 minutes.
In the first step, substrate 4 is 550 ℃ of down annealing 4.5 hours, 5 ℃ of following electrochemical etchings 40 seconds; In second step, the concentration of sulphuric acid soln is 14wt%, and once anodised temperature is 0 ℃, and anodizing time and electric current were respectively 3.5 hours and 6mA; In the 3rd step, the water-bath time is 45 minutes, and the concentration of sulphuric acid soln is 14wt%, and the temperature of two-step anodization is 0 ℃, and anodizing time and electric current were respectively 3 hours and 7mA; In the 4th step, water-bath 50 minutes; In the 5th step, removing aluminium base 40 solution is that concentration is the SnCl of 13wt%
4Solution, soak time are 6 hours; In the 6th step, the reaction times is 13 minutes; In the 9th step, depositing time is 15 minutes.
In the first step, substrate 4 is 650 ℃ of down annealing 5 hours, 10 ℃ of following electrochemical etchings 50 seconds; In second step, the concentration of sulphuric acid soln is 16wt%, and once anodised temperature is 6 ℃, and anodizing time and electric current were respectively 5 hours and 2mA; In the 3rd step, the water-bath time is 50 minutes, and the concentration of sulphuric acid soln is 16wt%, and the temperature of two-step anodization is 6 ℃, and anodizing time and electric current were respectively 5 hours and 2mA; In the 4th step, water-bath 60 minutes; In the 5th step, removing aluminium base 40 solution is that concentration is the SnCl of 16wt%
4Solution, soak time are 4 hours; In the 6th step, the reaction times is 16 minutes; In the 9th step, depositing time is 20 minutes.
Embodiment 4
Except that following difference, all the other operations of present embodiment are identical with embodiment 1 all:
In the 5th step, removing aluminium base 40 solution is that concentration is the Cupric Chloride Solution of 10wt%.
Embodiment 5
Except that following difference, all the other operations of present embodiment are identical with embodiment 2 all:
In the 5th step, removing aluminium base 40 solution is that concentration is the Cupric Chloride Solution of 13wt%.
Except that following difference, all the other operations of present embodiment are identical with embodiment 3 all:
In the 5th step, removing aluminium base 40 solution is that concentration is the Cupric Chloride Solution of 16wt%.
Claims (7)
1. one kind prepares the method for zinc sulfide quantum wire with template, it is characterized in that the concrete operations step:
The first step is cleaned substrate (4) with traditional method
Get a purity and be 99.999% aluminium flake, specification is 20mm * 20mm * 0.5mm, as substrate (4); Be placed on and carry out ultrasonic cleaning in the acetone, it is dry to put into baking oven after the cleaning, places nitrogen atmosphere again; 450 ℃～650 ℃ down annealing 4 hours～6 hours are carried out electrochemical etching then in volume ratio is 1: 4 perchloric acid and alcoholic acid mixing solutions, polish temperature is 0 ℃～10 ℃; Polishing time is 30 seconds～50 seconds, cleans substrate (4) surface with acid solution or alkaline solution at last;
A second step anodic oxidation
To put into the sulphuric acid soln that concentration is 12wt%～16wt% through the substrate (4) that the first step is handled; Under-6 ℃～6 ℃, carry out the anodic oxidation first time; Negative electrode and anode are respectively platinized platinum and substrate (4); Anodised voltage, electric current and time are respectively 20 volts, 1mA～10mA and 2 hours～5 hours, on the front and back of substrate (4), form the straight tackling layer respectively
(3) and backside barrier layer (5); Straight tackling layer (3) and backside barrier layer (5) are the alumina layers that does not contain microwell array; Then on straight tackling layer (3) and backside barrier layer (5), form front alumina layer (2) and back side alumina layer (6), front alumina layer respectively
(2) and back side alumina layer (6) be the alumina layer that contains microwell array, but the microwell array that an anodic oxidation forms, the pore size of its micropore is even inadequately, the arrangement of its array is neat inadequately, need carry out two-step anodization;
The 3rd step two-step anodization
To put into by phosphoric acid, chromic acid and water through the substrate (4) that second step handled and mix mixing liquid; Phosphoric acid: chromic acid: the weight ratio of water is 6: 1.8: 92.2,65 ℃ of water-baths 40 minutes～60 minutes, deoxidation aluminium lamination; This alumina layer comprises front alumina layer (2), straight tackling layer (3), backside barrier layer (5) and back side alumina layer (6); Again under-6 ℃～6 ℃,, concentration carries out the anodic oxidation second time in being the sulphuric acid soln of 12wt%～15wt%, and negative electrode and anode are respectively platinized platinum and the substrate (4) handled through deoxidation aluminium film; Anodised voltage, electric current and time are respectively 20 volts, 2mA～10mA and 2 hours～5 hours; On the front and back of substrate (4), form straight tackling layer (3) and backside barrier layer (5) respectively, on straight tackling layer (3) and backside barrier layer (5), form front alumina layer (2) and back side alumina layer (6) then respectively, compare with an anodic oxidation in second step; The microwell array that two-step anodization forms; The aperture of its micropore is 8～15nm, and size is even, the marshalling of its array;
The 4th step was removed the alumina layer on substrate (4) back side
Go aluminium base anchor clamps (7) to process, comprise top board (8) and base plate (11), have hole (9) in the central part office of top board (8) with tetrafluoroethylene; Hole (9) is that diameter is the circular hole of 7mm; On four jiaos of top board (8) and base plate (11) screw (10) is arranged respectively, during use, top board (8) and base plate (11) are fixed with four screws; Substrate (4) is clamped between top board (8) and the base plate (11); To be clamped in the aluminium base anchor clamps (7) through the substrate (4) that the 3rd step handled, outside only the centre portions at substrate (4) back side is exposed to, again clamping substrate (4) gone aluminium base anchor clamps (7) to put into by phosphoric acid, chromic acid and water to mix mixing liquid; Phosphoric acid: chromic acid: the weight ratio of water is 6: 1.8: 92.2; The alumina layer on the centre portions at substrate (4) back side is removed in 65 ℃ of water-baths 40 minutes～60 minutes, and this alumina layer comprises back side alumina layer (6) and backside barrier layer (5);
The 5th step was gone to aluminium base (40)
Substrate (4) is put into the SnCl that concentration is 10wt%～16wt% with its aluminium base anchor clamps (7) that go of clamping
4In solution or the Cupric Chloride Solution, soaked 4 hours～8 hours, remove aluminium base (40), aluminium base (40) are exactly the centre portions of substrate (4);
The 6th step was removed straight tackling layer (3)
Substrate (4) is put into the phosphoric acid that concentration is 6wt% with its aluminium base anchor clamps (7) that go of clamping; 30 ℃ were reacted 10 minutes～16 minutes down; Remove straight tackling layer (3); Unload down aluminium base anchor clamps (7), obtain containing the substrate (4) of front alumina layer (2), promptly contain the alumina layer nano-form (12) of microwell array;
The 7th step sputter Au electrode
With the back spatter layer of Au electrode of the 6th aluminium oxide nano-form that contains microwell array (12) that make of step, thickness is 200 nanometers;
The 8th step obtain solution
At room temperature, preparation contains 7.5gL
-1ZnCl
2And 6.1gL
-1The dimethyl sulphoxide solution of sulphur simple substance;
The 9th step dc electrodeposition
The aluminium base anchor clamps (7) that go of the alumina layer nano-form (12) that contains microwell array that clamping was handled through the 7th step are put into the solution of the 8th step preparation, under 120 ℃, carry out dc electrodeposition, and current density is 6.62mA/cm
2The alumina layer nano-form (12) that contains microwell array that anode and negative electrode are respectively platinized platinum and handle through the 7th step deposit 10 minutes～20 minutes, formation zinc sulfide quantum wire in the micropore (1) of the microwell array of this nano-form; Take out this nano-form; Use dimethyl sulphoxide solution, acetone and deionized water rinsing clean successively, seasoning under the room temperature makes the zinc sulfide quantum wire in the microwell array that is stored in the alumina layer nano-form (12) that contains microwell array.
2. according to claim 1ly prepare the method for zinc sulfide quantum wire with template, it is characterized in that, in the first step, substrate (4) is 450 ℃ of annealing 4 hours down, 0 ℃ of following electrochemical etching 30 seconds; In second step, the concentration of sulphuric acid soln is 12wt%, and once anodised temperature is-6 ℃, and anodizing time and electric current were respectively 2 hours and 10mA; In the 3rd step, the water-bath time is 40 minutes, and the concentration of sulphuric acid soln is 12wt%, and the temperature of two-step anodization is-6 ℃, and anodizing time and electric current were respectively 2 hours and 10mA; In the 4th step, water-bath 40 minutes; In the 5th step, the solution that goes to aluminium base (40) is that concentration is the SnCl of 10wt%
4Solution, soak time are 8 hours; In the 6th step, the reaction times is 10 minutes; In the 9th step, depositing time is 10 minutes.
3. according to claim 2ly prepare the method for zinc sulfide quantum wire, it is characterized in that in the 5th step, concentration is the SnCl of 10wt% with template
4Solution replaces with the Cupric Chloride Solution that concentration is 10wt%.
4. according to claim 1ly prepare the method for zinc sulfide quantum wire with template, it is characterized in that, in the first step, substrate (4) is 550 ℃ of annealing 4.5 hours down, 5 ℃ of following electrochemical etchings 40 seconds; In second step, the concentration of sulphuric acid soln is 14wt%, and once anodised temperature is 0 ℃, and anodizing time and electric current were respectively 3.5 hours and 6mA; In the 3rd step, the water-bath time is 45 minutes, and the concentration of sulphuric acid soln is 14wt%, and the temperature of two-step anodization is 0 ℃, and anodizing time and electric current were respectively 3 hours and 7mA; In the 4th step, water-bath 50 minutes; In the 5th step, the solution that goes to aluminium base (40) is that concentration is the SnCl of 13wt%
4Solution, soak time are 6 hours; In the 6th step, the reaction times is 13 minutes; In the 9th step, depositing time is 15 minutes.
5. according to claim 4ly prepare the method for zinc sulfide quantum wire, it is characterized in that in the 5th step, concentration is the SnCl of 13wt% with template
4Solution replaces with the Cupric Chloride Solution that concentration is 13wt%.
6. according to claim 1ly prepare the method for zinc sulfide quantum wire with template, it is characterized in that, in the first step, substrate (4) is 650 ℃ of annealing 5 hours down, 10 ℃ of following electrochemical etchings 50 seconds; In second step, the concentration of sulphuric acid soln is 16wt%, and once anodised temperature is 6 ℃, and anodizing time and electric current were respectively 5 hours and 2mA; In the 3rd step, the water-bath time is 50 minutes, and the concentration of sulphuric acid soln is 15wt%, and the temperature of two-step anodization is 6 ℃, and anodizing time and electric current were respectively 5 hours and 2mA; In the 4th step, water-bath 60 minutes; In the 5th step, the solution that goes to aluminium base (40) is that concentration is the SnCl of 16wt%
4Solution, soak time are 4 hours; In the 6th step, the reaction times is 16 minutes; In the 9th step, depositing time is 20 minutes.
7. according to claim 6ly prepare the method for zinc sulfide quantum wire, it is characterized in that in the 5th step, concentration is the SnCl of 16wt% with template
4Solution replaces with the Cupric Chloride Solution that concentration is 16wt%.
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