CN104016300A - Method for constructing silver film trap structure on metal surface by utilizing PS microspheres as template - Google Patents
Method for constructing silver film trap structure on metal surface by utilizing PS microspheres as template Download PDFInfo
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Abstract
The invention relates to a method for constructing a silver film trap structure on a metal surface by utilizing PS microspheres as a template. In a conventional process for preparing a metal nano-porous array, the equipment requirement is strict, the cost is high, or the template morphology needs to be subjected to earlier-stage development, and time consumption is high. The method comprises the following steps: self-assembling PS microspheres on the metal surface through an evaporation deposition method; with the PS microspheres as the template, plating silver in gaps between the PS microspheres by utilizing an electrochemical deposition method, and finally, removing the PS microsphere template by using an organic solvent, and constructing the silver film trap structure on the metal surface. The method is high in operability, the constructed silver film trap structure is high in crystalline quality, and impurity residues are avoided. Meanwhile, the process for self-assembling the PS microspheres on the metal surface is simple, the repeatability is high, and the secondary electron emission coefficient on the metal surface can be reduced to be over 25 percent.
Description
Technical field
the present invention relates to a kind of method of constructing silverskin structure of trap in metal surface, be specifically related to a kind of PS of utilization microballoon and in metal surface, construct the method for silverskin structure of trap for template.
Background technology
Silverskin structure of trap, is generally exactly at the constructed nanometer porous structure going out of argent film surface, i.e. so-called nano-pore array structure.Utilize metal nano-void array structure can effectively excite and regulate metal surface plasma resonance body (SPR) phenomenon, thereby inspire some special optical effects, such as superpower smooth reflected effect (EOT), surface Raman enhancement effect (SERS), surface, strengthen fluorescent effect (SEFS), can be in aspect performance application such as biochemistry detection sensor, nanocomposite optical device and solar cells.
At present, a lot of about the preparation technology of different-shape metal nano-void array, mainly can be divided into etching method and template.Wherein, more representational in etching method have focused-ion-beam lithography (FIB) and an electron beam lithography (EBL), and it is mainly to utilize high energy ion beam or electron beam directly at sample surfaces, to etch needed pore space structure.Adopt etching method to prepare nano-pore array structure and there is the advantages such as favorable reproducibility, the size that also can control well nano-pore and pattern, in the preparation of optical analysis substances and biology sensor, brought into play important effect.But the method also exists the shortcoming that equipment requirement is harsh, cost is high, etch period is long, has limited it in the application of preparing on a large scale in nanohole array.Adopt template synthesis metal nano-void array, mainly to utilize to have that some cycles is arranged and the nanosphere of pattern or the polymer mask of patterning are made template, by certain deposition technique or lithographic method, at stencil apertures plated metal or carry out etching and remove template, finally obtain having the nano-pore structure of certain pattern, size and periodic arrangement.What wherein, template was relatively more conventional is Nanosphere lithography technique (NSL) and nanometer embossing (NIL).Template technique is simple, sample surfaces porosity and cost have greatly been improved relatively cheap, made up to a certain extent etching method at nanohole array the deficiency aspect preparing, but the method also exists simultaneously, need in advance the pattern of template and size to be carried out to the problems such as systematic research and design, elapsed time length, need badly in practice and find a kind of method for preparing template easily and efficiently to enhance productivity.
In addition, the method of chemical solution corrosion also occurs, silver coated aluminum alloy print is carried out to anodized in acidic electrolysis bath, on print surface, form loose structure, then utilize the method for chemical solution corrosion to increase the bore in hole, at the gold of inner surface sputter one deck good conductivity in hole or silver-colored, finally form nano-pore array structure again.Use the method for electrochemical corrosion to go out loose structure in print surface etch, with respect to adopting high energy ion beam or electron beam lithography, have equipment simple, cost is low, implements the advantages such as convenient.But electrochemical corrosion is carried out along the crystal boundary surface of the material that is corroded often, and general metal material itself is all anisotropic, therefore adopt the method etching nano-pore array structure out also will show anisotropy, size and distributing homogeneity that can not nano-pore array structure that fine control forms.
Successively by operations such as ultrasonic cleaning, spin coating, baking, exposure, baking, development treatment and etching liquid etchings, also can realize constructing of microwave component rule of surface nano-pore array structure, but the method adopts the photoresist of patterning to make template carries out selective etch to microwave component, operation sequence is more, and etching process is uncontrollable equally, size that can not nano-pore array structure that fine control forms.
Summary of the invention
The object of this invention is to provide a kind of PS of utilization microballoon and in metal surface, construct the method for silverskin structure of trap for template, can effectively improve porosity and the depth-to-width ratio of metal surface, can be used for suppressing metal surface secondary.
The technical solution adopted in the present invention is:
Utilize PS microballoon in metal surface, to construct the method for silverskin structure of trap for template, it is characterized in that:
By following steps, realized:
Step 1: take PS microballoon, added in absolute ethyl alcohol-water mixed solution, make PS microballoon dispersion liquid after ultrasonic dispersion 30min; Then, get two coupons and be fixed in the measuring cup of 40 * 25mm, add the PS microballoon dispersion liquid preparing to just flooding print; Finally, whole device is placed in to baking oven and treats that liquid evaporation is dry, take out print, use the clean rear 100 ℃ of oven dry of distilled water flushing, obtain the print that area load has PS microballoon;
Step 2: area load is had to the print of PS microballoon as working electrode, be connected to the negative electrode of constant voltage stabilized current supply; Separately get the silver foil of homalographic as sacrificial electrode, be connected to the anode of constant voltage stabilized current supply, under constant-pressure conditions, carry out silver-plated; After silver-plated, adopt organic solvent to carry out corrosion treatment to print, then clean, be dried, can go out silverskin structure of trap at coupon surface construction.
In step 1, the diameter of PS microballoon is 500nm, and the mass concentration of PS microballoon dispersion liquid is 0.01%-0.05%.
In step 1, in absolute ethyl alcohol-water mixed solution, the volume ratio of absolute ethyl alcohol and deionized water is 3:7-10:0.
In step 1, coupon is of a size of 24 * 12 * 1mm, and two prints dock along the limit of 12mm, and are 90 °, and angle is fixed in the measuring cup of 40 * 25mm.
In step 1, the evaporating temperature of baking oven is 25-85 ℃.
In step 2, adopt the deposition voltage of 0.5-1.0V to carry out silver-plated, the silver-plated time is 10-20min, after the 10min of interval, carry out silver-platedly for the second time, the silver-plated time is 0-20min for the second time, absolute ethyl alcohol-aqueous solution that silver-plated electrolyte is silver nitrate, the mass concentration of silver nitrate is 1.16g/L, and the volume ratio of absolute ethyl alcohol and deionized water is 1:1-4:1.
In step 2, organic solvent is selected from oxolane, tetrachloromethane, and the corrosion treatment time is 3 hours.
In step 2, silver-plated two interelectrode vertical ranges are 1.0-3.0cm.
The present invention has the following advantages:
(1) the present invention adopts evaporation deposition method at metal surface self assembly PS microballoon, and technique is simple, and cost is low, repeatable strong, is convenient to large-scale production.
(2) the present invention be take PS microballoon and is constructed silverskin structure of trap as template, and crystal mass is high, and free from admixture is residual, when when suppressing metal surface secondary, can effectively metal surface secondary electron yield be reduced more than 25%.
Accompanying drawing explanation
Fig. 1 is the SEM figure after coupon surface self-organization PS microballoon;
Fig. 2 is the SEM figure after PS microsphere template gap is silver-plated;
Fig. 3 is the SEM figure that removes the silverskin structure of trap obtaining after PS microsphere template;
Fig. 4 constructs the forward and backward XRD of silverskin structure of trap figure for take silver coated aluminum alloy print as substrate;
Fig. 5 is the SEY characteristic curve after silver coated aluminum alloy print surface construction silverskin structure of trap, and wherein, a point, No. two points, No. three points refer to respectively three random different test points of print surface.
The specific embodiment
Below in conjunction with the specific embodiment, the present invention will be described in detail.
The involved in the present invention PS microballoon that utilizes is constructed the method for silverskin structure of trap for template in metal surface, by following steps, realized:
Step 1: take PS microballoon, added in absolute ethyl alcohol-water mixed solution, make PS microballoon dispersion liquid after ultrasonic dispersion 30min; Then, get two coupons and be fixed in the measuring cup of 40 * 25mm, add the PS microballoon dispersion liquid preparing to just flooding print; Finally, whole device is placed in to baking oven and treats that liquid evaporation is dry, take out print, use the clean rear 100 ℃ of oven dry of distilled water flushing, obtain the print that area load has PS microballoon.
In step 1:
The diameter of PS microballoon is 500nm, and the mass concentration of PS microballoon dispersion liquid is 0.01%-0.05%;
In absolute ethyl alcohol-water mixed solution, the volume ratio of absolute ethyl alcohol and deionized water is 3:7-10:0;
Coupon is of a size of 24 * 12 * 1mm, and two prints dock along the limit of 12mm, and are 90 °, and angle is fixed in the measuring cup of 40 * 25mm;
The evaporating temperature of baking oven is 25-85 ℃.
Step 2: area load is had to the print of PS microballoon as working electrode, be connected to the negative electrode of constant voltage stabilized current supply; Separately get the silver foil of homalographic as sacrificial electrode, be connected to the anode of constant voltage stabilized current supply, under constant-pressure conditions, carry out silver-plated; After silver-plated, adopt organic solvent to carry out corrosion treatment to print, then clean, be dried, can go out silverskin structure of trap at coupon surface construction.
In step 2:
Adopt the deposition voltage of 0.5-1.0V to carry out silver-plated, the silver-plated time is 10-20min, after the 10min of interval, carry out silver-plated for the second time, the silver-plated time is 0-20min for the second time, silver-plated electrolyte is the absolute ethyl alcohol-aqueous solution of silver nitrate, and the mass concentration of silver nitrate is 1.16g/L, and the volume ratio of absolute ethyl alcohol and deionized water is 1:1-4:1;
Organic solvent is selected from oxolane, tetrachloromethane, and the corrosion treatment time is 3 hours;
Silver-plated two interelectrode vertical ranges are 1.0-3.0cm.
Embodiment 1:
Step 1: take PS microballoon, added in absolute ethyl alcohol-water mixed solution, make PS microballoon dispersion liquid after ultrasonic dispersion 30min; Then, get two coupons and be fixed in the measuring cup of 40 * 25mm, add the PS microballoon dispersion liquid preparing to just flooding print; Finally, whole device is placed in to baking oven and treats that liquid evaporation is dry, take out print, use the clean rear 100 ℃ of oven dry of distilled water flushing, obtain the print that area load has PS microballoon.
In step 1:
The diameter of PS microballoon is 500nm, and the mass concentration of PS microballoon dispersion liquid is 0.01%%;
In absolute ethyl alcohol-water mixed solution, the volume ratio of absolute ethyl alcohol and deionized water is 3:7;
Coupon is of a size of 24 * 12 * 1mm, and two prints dock along the limit of 12mm, and are 90 °, and angle is fixed in the measuring cup of 40 * 25mm;
The evaporating temperature of baking oven is 25 ℃.
Step 2: area load is had to the print of PS microballoon as working electrode, be connected to the negative electrode of constant voltage stabilized current supply; Separately get the silver foil of homalographic as sacrificial electrode, be connected to the anode of constant voltage stabilized current supply, under constant-pressure conditions, carry out silver-plated; After silver-plated, adopt organic solvent to carry out corrosion treatment to print, then clean, be dried, can go out silverskin structure of trap at coupon surface construction.
In step 2:
The deposition voltage of employing 0.5V carries out silver-plated, and the silver-plated time is 10min, absolute ethyl alcohol-aqueous solution that silver-plated electrolyte is silver nitrate, and the mass concentration of silver nitrate is 1.16g/L, the volume ratio of absolute ethyl alcohol and deionized water is 1:1;
Organic solvent is oxolane, and the corrosion treatment time is 3 hours;
Silver-plated two interelectrode vertical ranges are 1.0cm.
Embodiment 2:
Step 1: take PS microballoon, added in absolute ethyl alcohol-water mixed solution, make PS microballoon dispersion liquid after ultrasonic dispersion 30min; Then, get two coupons and be fixed in the measuring cup of 40 * 25mm, add the PS microballoon dispersion liquid preparing to just flooding print; Finally, whole device is placed in to baking oven and treats that liquid evaporation is dry, take out print, use the clean rear 100 ℃ of oven dry of distilled water flushing, obtain the print that area load has PS microballoon.
In step 1:
The diameter of PS microballoon is 500nm, and the mass concentration of PS microballoon dispersion liquid is 0.03%;
In absolute ethyl alcohol-water mixed solution, the volume ratio of absolute ethyl alcohol and deionized water is 7:3;
Coupon is of a size of 24 * 12 * 1mm, and two prints dock along the limit of 12mm, and are 90 °, and angle is fixed in the measuring cup of 40 * 25mm;
The evaporating temperature of baking oven is 55 ℃.
Step 2: area load is had to the print of PS microballoon as working electrode, be connected to the negative electrode of constant voltage stabilized current supply; Separately get the silver foil of homalographic as sacrificial electrode, be connected to the anode of constant voltage stabilized current supply, under constant-pressure conditions, carry out silver-plated; After silver-plated, adopt organic solvent to carry out corrosion treatment to print, then clean, be dried, can go out silverskin structure of trap at coupon surface construction.
In step 2:
Adopt the deposition voltage of 0.7V to carry out silver-plated, the silver-plated time is 15min, after the 10min of interval, carry out silver-plated for the second time, the silver-plated time is 10min for the second time, silver-plated electrolyte is the absolute ethyl alcohol-aqueous solution of silver nitrate, and the mass concentration of silver nitrate is 1.16g/L, and the volume ratio of absolute ethyl alcohol and deionized water is 2:1;
Organic solvent is chosen oxolane, and the corrosion treatment time is 3 hours;
Silver-plated two interelectrode vertical ranges are 2.0cm.
Embodiment 3:
Step 1: take PS microballoon, added in absolute ethyl alcohol-water mixed solution, make PS microballoon dispersion liquid after ultrasonic dispersion 30min; Then, get two coupons and be fixed in the measuring cup of 40 * 25mm, add the PS microballoon dispersion liquid preparing to just flooding print; Finally, whole device is placed in to baking oven and treats that liquid evaporation is dry, take out print, use the clean rear 100 ℃ of oven dry of distilled water flushing, obtain the print that area load has PS microballoon.
In step 1:
The diameter of PS microballoon is 500nm, and the mass concentration of PS microballoon dispersion liquid is 0.05%;
In absolute ethyl alcohol-water mixed solution, the volume ratio of absolute ethyl alcohol and deionized water is 10:0, does not namely add deionized water, only adds absolute ethyl alcohol;
Coupon is of a size of 24 * 12 * 1mm, and two prints dock along the limit of 12mm, and are 90 °, and angle is fixed in the measuring cup of 40 * 25mm;
The evaporating temperature of baking oven is 85 ℃.
Step 2: area load is had to the print of PS microballoon as working electrode, be connected to the negative electrode of constant voltage stabilized current supply; Separately get the silver foil of homalographic as sacrificial electrode, be connected to the anode of constant voltage stabilized current supply, under constant-pressure conditions, carry out silver-plated; After silver-plated, adopt organic solvent to carry out corrosion treatment to print, then clean, be dried, can go out silverskin structure of trap at coupon surface construction.
In step 2:
Adopt the deposition voltage of 1.0V to carry out silver-plated, the silver-plated time is 20min, after the 10min of interval, carry out silver-plated for the second time, the silver-plated time is 20min for the second time, silver-plated electrolyte is the absolute ethyl alcohol-aqueous solution of silver nitrate, and the mass concentration of silver nitrate is 1.16g/L, and the volume ratio of absolute ethyl alcohol and deionized water is 4:1;
Organic solvent is chosen tetrachloromethane, and the corrosion treatment time is 3 hours;
Silver-plated two interelectrode vertical ranges are 3.0cm.
Fig. 1 is the SEM figure after coupon surface self-organization PS microballoon, can find out that the method in employing the present invention is carried out the self assembly of PS microballoon, and PS microballoon is substantially individual layer on coupon surface and is uniformly distributed.Fig. 2 is the SEM figure of PS microsphere template gap after silver-plated, by the contrast of Fig. 1 and Fig. 2, can find out, silver-platedly with sheet form, is interspersed in PS microballoon gap, and size is much larger than PS microballoon.Fig. 3 is the SEM figure that removes gained silverskin structure of trap after PS microsphere template, can find out that PS microballoon removes substantially completely, and the roughness of silverskin structure of trap is larger.Fig. 4 constructs the forward and backward XRD of silverskin structure of trap figure for take silver coated aluminum alloy print as substrate, the relative silver coated aluminum alloy substrate of silverskin structure of trap that known employing the method is constructed, orientation along (200) crystal face improves, but there is no the appearance of other impurity peaks, illustrate that constructed silverskin trap has high crystal mass.Fig. 5 is that silver coated aluminum alloy surface is constructed the SEY characteristic curve after silverskin structure of trap, at silver coated aluminum alloy surface, randomly draw three test points as shown in Figure 5, its SEY maximum average out to 1.64, has reduced by 26.8% with respect to silver coated aluminum alloy surface SEY maximum 2.24.
It is cited that content of the present invention is not limited to embodiment, and the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading description of the present invention, is claim of the present invention and contains.
Claims (8)
1. utilize PS microballoon in metal surface, to construct the method for silverskin structure of trap for template, it is characterized in that:
By following steps, realized:
Step 1: take PS microballoon, added in absolute ethyl alcohol-water mixed solution, make PS microballoon dispersion liquid after ultrasonic dispersion 30min; Then, get two coupons and be fixed in the measuring cup of 40 * 25mm, add the PS microballoon dispersion liquid preparing to just flooding print; Finally, whole device is placed in to baking oven and treats that liquid evaporation is dry, take out print, use the clean rear 100 ℃ of oven dry of distilled water flushing, obtain the print that area load has PS microballoon;
Step 2: area load is had to the print of PS microballoon as working electrode, be connected to the negative electrode of constant voltage stabilized current supply; Separately get the silver foil of homalographic as sacrificial electrode, be connected to the anode of constant voltage stabilized current supply, under constant-pressure conditions, carry out silver-plated; After silver-plated, adopt organic solvent to carry out corrosion treatment to print, then clean, be dried, can go out silverskin structure of trap at coupon surface construction.
2. the PS of utilization microballoon according to claim 1 is constructed the method for silverskin structure of trap for template in metal surface, it is characterized in that:
In step 1, the diameter of PS microballoon is 500nm, and the mass concentration of PS microballoon dispersion liquid is 0.01%-0.05%.
3. the PS of utilization microballoon according to claim 2 is constructed the method for silverskin structure of trap for template in metal surface, it is characterized in that:
In step 1, in absolute ethyl alcohol-water mixed solution, the volume ratio of absolute ethyl alcohol and deionized water is 3:7-10:0.
4. the PS of utilization microballoon according to claim 3 is constructed the method for silverskin structure of trap for template in metal surface, it is characterized in that:
In step 1, coupon is of a size of 24 * 12 * 1mm, and two prints dock along the limit of 12mm, and are 90 °, and angle is fixed in the measuring cup of 40 * 25mm.
5. the PS of utilization microballoon according to claim 4 is constructed the method for silverskin structure of trap for template in metal surface, it is characterized in that:
In step 1, the evaporating temperature of baking oven is 25-85 ℃.
6. the PS of utilization microballoon according to claim 5 is constructed the method for silverskin structure of trap for template in metal surface, it is characterized in that:
In step 2, adopt the deposition voltage of 0.5-1.0V to carry out silver-plated, the silver-plated time is 10-20min, after the 10min of interval, carry out silver-platedly for the second time, the silver-plated time is 0-20min for the second time, absolute ethyl alcohol-aqueous solution that silver-plated electrolyte is silver nitrate, the mass concentration of silver nitrate is 1.16g/L, and the volume ratio of absolute ethyl alcohol and deionized water is 1:1-4:1.
7. the PS of utilization microballoon according to claim 6 is constructed the method for silverskin structure of trap for template in metal surface, it is characterized in that:
In step 2, organic solvent is selected from oxolane, tetrachloromethane, and the corrosion treatment time is 3 hours.
8. the PS of utilization microballoon according to claim 7 is constructed the method for silverskin structure of trap for template in metal surface, it is characterized in that:
In step 2, silver-plated two interelectrode vertical ranges are 1.0-3.0cm.
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