CN103668130A - Preparation method of metal nanostructure - Google Patents
Preparation method of metal nanostructure Download PDFInfo
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- CN103668130A CN103668130A CN201210360802.4A CN201210360802A CN103668130A CN 103668130 A CN103668130 A CN 103668130A CN 201210360802 A CN201210360802 A CN 201210360802A CN 103668130 A CN103668130 A CN 103668130A
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Abstract
The invention discloses a preparation method of a metal nanostructure. The preparation method comprises the steps of (1) manufacturing a mask plate; (2) providing a clean and dry base plate, uniformly coating a positive ultraviolet photoresist on the base plate, and pre-baking to ensure that the positive ultraviolet photoresist is solidified to form a photoresist base plate; (3) overlapping the mask plate on the photoresist base plate, and performing exposure, development, residual adhesive removal and hardening under ultraviolet light to obtain a forming mold with shape grooves of a nanostructure graph; (4) depositing a metal in the forming mold by adopting a chemical synthetic method; (5) soaking the forming mold deposited with the metal in an acetone solution, and performing ultrasonic adhesive removal to obtain the metal nanostructure of the nanostructure graph. The preparation method disclosed by the invention is simple in process and high in efficiency; the shape, size and position of the prepared metal nanostructure can be accurately controlled, and the light extraction efficiency and light absorption efficiency of a metal nanostructure material are effectively improved.
Description
Technical field
The present invention relates to a kind of Ultrastructural preparation method, especially a kind of preparation method of metal Nano structure.
Background technology
Metal Nano structure material is a large study hotspot of optical field in recent years, because its surface plasma can be by the very special optical property of generation that light wave excites, thereby at photochemical catalysis, nanometer integrated photonics, optical sensing, biomarker, medical imaging, solar cell, and the field such as surface enhanced Raman spectroscopy is with a wide range of applications.
Its equal yardstick in 1～100nm in the arbitrary dimension of three-dimensional space of metal Nano structure material general requirement, its shape, size, composition, structure have determined the performance of metal nano material to a great extent.Accurately control shape, size, the position of metal nano material, for utilizing metal Nano structure excitating surface plasma excimer, improve the light extraction efficiency of luminescent material and the efficiency of light absorption of solar cell and have very important significance.
People generally adopt chemical process to carry out the synthetic of metal nanoparticle at present; for example chemical reduction method, photoreduction met hod, irradiation method, polyvalent alcohol method, chemical deposition; these methods can be prepared metal nanoparticle; although can be by controlling the size that the ratio of reactant and reaction times controls metal Nano structure; but because the direction of growth and the position of resultant is all random; thereby metal nanoparticle shape prepared by these methods differs; different sizes; and arrange very chaoticly, affected the optical property of metal Nano structure material.
In recent years, the method that has researchist to propose to adopt photoetching technique to combine with deposition technique is prepared shape, size, the controlled metal Nano structure (for example patent 200910226780.0) in position, this method is first prepared non-fine and close arrangement of the orderly silica nanosphere of individual layer at silicon chip, evaporation or sputtering metal membrane thereon again, as etching mask, then silicon chip is corroded, obtain nano-structure array template, finally metal refining particle in template, obtains metal Nano structure.This method has overcome traditional chemical method to be prepared metal nanoparticle shape and differs, different sizes, and the defect of fall into disarray, the metal Nano structure shape of preparation, size, position are more controlled.But because preparation process requires first to deposit the film of layer, and film growth will be passed through the process that the alligatoring on absorption, nucleation, Cheng Dao, island merges, the relatively coarse injustice in thinner film (thickness is less than 100nm) surface, thereby it all lacks accuracy to the shape of metal Nano structure and big or small control, the shape of the metal Nano structure of preparation and big or small homogeneity can not get ensureing, have affected equally light extraction efficiency and the efficiency of light absorption of metal Nano structure material.
Summary of the invention
The object of the invention is to the existing method of preparing metal Nano structure with photoetching technique to improve, a kind of preparation method of metal Nano structure is provided, this preparation method's technique is simple, efficiency is high, can prepare according to actual needs the metal Nano structure that shape, size, position all can accurately be controlled, identical, the big or small homogeneous of metal Nano structure shape making, arrangement in order, have improved light extraction efficiency and the efficiency of light absorption of metal Nano structure material effectively.
The present invention solves the problems of the technologies described above adopted scheme:
A preparation method for metal Nano structure, comprises the following steps:
(1) provide clean substrate, and on substrate, make required nanostructure figure, form mask plate, on described substrate, have the position of figure to UV transparent;
(2) provide clean dry substrate, and on substrate, evenly apply positivity ultraviolet photoresist, front baking, makes the adhesive curing of positivity ultraviolet photolithographic, forms photoresist material substrate;
(3) described mask plate is stacked on described photoresist material substrate, after exposing, develop, go cull post bake under ultraviolet ray, obtains the forming mould with described nanostructure graphics shape groove;
(4) adopt chemical synthesis metal refining in described forming mould;
(5) the described forming mould that has deposited metal is immersed in acetone soln, ultrasonic depolymerization, obtains the metal Nano structure of described nanostructure figure.
Preferably, the material of the described substrate of step (1) is wolfram steel, ferric oxide or chromium.
Preferably, the nanostructure figure that step (1) is described, adopts copier, Laser pattern generation system or electron beam pattern generator to draw, or adopts X ray to scribe.
Preferably, the described substrate of step (2) is glass substrate, silicon substrate or gallium oxide substrate.
Particularly, the clean drying operation of the described substrate of step (2) is: use successively chromic acid scavenging solution, clean-out system and washed with de-ionized water, then substrate is put into baking oven, with dry 10～15 minutes of the temperature of 150～200 ° of C.
Preferably, the substrate that step (2) is described, its sizes and shape is identical with described mask plate.Thereby guarantee that mask plate and substrate can be completely overlapping, the figure on it can precise positioning to described substrate.
Wherein, the positivity ultraviolet photoresist that step (2) is described, its coating thickness can be determined according to the size of described metal Nano structure.Preferably, the coating thickness of described positivity ultraviolet photoresist is 20～50nm.
Preferably, the described positivity ultraviolet photoresist of step (2) GP18 series U.V. positive photoresist, SUN-115P ultraviolet positive photoresist, or take poly-N-(p-carboxyl phenyl) Methacrylamide of the multipolymer ultraviolet positive photoresist that N-phenylmaleimide is main raw altogether.
Preferably, the front baking described in step (2) is for to put into incubator by the described substrate that is coated with ultraviolet photoresist, with 50～80 ℃ of bakings 1～2 hour.
Preferably, the described development of step (3) is soaked for the photoresist material substrate through overexposure is put into developing solution, and the photoresist material through ultraviolet exposure on substrate is dissolved by the developing.The object of developing is to form the groove of required nanostructure graphics shape in photoresist material.
Preferably, step (3) is described, and to remove cull be that the photoresist material substrate after developing is placed in plasma etching machine to etching 10～15 minutes.In developing process, may occur that part is not dissolved completely through the photoresist material of ultraviolet exposure, therefore can be by going cull that this part photoresist material is removed, thereby guarantee homogeneity and the accuracy of groove, and then prevent that the metal Nano structure shape size of preparation is uneven.
Preferably, the described post bake of step (3) for by described through going the photoresist material substrate of cull to put into incubator, with 60～80 ℃ of bakings 1～2 hour, the photoresist material on substrate is solidified.Softening through the photoresist material developing, expand, the adhesion between glued membrane and substrate declines, and the object of post bake is to make residual photoresist solvent all volatilize, improve photoresist material and the adhesion of substrate surface and the resistance to corrosion of photoresist material, remove remaining developing solution and water simultaneously.
Preferably, the described chemical synthesis of step (4) is chemical reduction method, photoreduction met hod, irradiation method or polyvalent alcohol method.
Wherein, chemical reduction method for to add reductive agent, to generate metal nanoparticle in metal salt solution; Photoreduction met hod be by photoresist material substrate immersion to metal salt solution, with ultraviolet source induction, generate metal nanoparticle; Irradiation method is to utilize gamma-rays to make water molecules ionization produce the hydrated electron of strong reducing property, thereby metal ion is reduced to metal nanoparticle; Polyvalent alcohol method for to add polyvalent alcohol, polyvalent alcohol to be first oxidized to glycollic aldehyde under heating condition in metal salt solution, and aldehyde radical is reduced to metal nanoparticle by metal ion.
Preferably, the described metal of step (4) is silver.Silver nanostructured being directly used in made solar cell surface antireflection structure.
Preferably, the ultrasonic depolymerization that step (5) is described, ultrasonic time is 20～40 minutes.
Wherein, the metal Nano structure that step (5) is described, its shape can be controlled by the nanostructure figure on substrate described in step 1.Preferably, the metal Nano structure described in step 5, is the array structure of square, rectangular parallelepiped or rectangular pyramid.
Wherein, the metal Nano structure that step (5) is described, wherein large I is controlled by the size of the nanostructure figure on substrate described in step 1, and thickness can be controlled by concentration and the reaction times of reactant in chemical synthesis.Preferably, the metal Nano structure described in step 5, is the array structure of the square of length of side 40nm.
The present invention first will form the groove of required nanostructure graphics shape by photoetching technique on photoresist material substrate, forming mould as metal nanoparticle, then electroless plating metallics in described groove, finally remove the photoresist material on substrate, formed the metal Nano structure that shape, size, position all can accurately be controlled.The shape of metal Nano structure, size and position can be controlled by being adjusted to shape, size, the position of the groove on mould.
Than prior art, preparation technology of the present invention is simpler, and efficiency is high; Without first depositing metal films, prevented the impact that the relatively coarse injustice in metallic film surface is brought metal Nano structure, the metal Nano structure shape making, size, position all can accurately be controlled, thereby effectively utilize metal Nano structure excitating surface plasma excimer, improve light extraction efficiency and the efficiency of light absorption of metal Nano structure material.
Accompanying drawing explanation
In order to be illustrated more clearly in technical scheme of the present invention, to the accompanying drawing of required use in embodiment be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the vertical view of the metal Nano structure of the embodiment of the present invention one preparation;
Fig. 2 is the perspective view of the metal Nano structure of the embodiment of the present invention one preparation;
Fig. 3 is the perspective view of the metal Nano structure of the embodiment of the present invention two preparations;
Embodiment
Below in conjunction with the accompanying drawing in embodiment of the present invention, the technical scheme in embodiment of the present invention is clearly and completely described.
Embodiment mono-
A preparation method for metal Nano structure, comprises the following steps:
(1) provide clean substrate, and on substrate, make required nanostructure figure, form mask plate, on described substrate, have the position of figure to UV transparent;
The wolfram steel substrate of selecting the thick 0.5cm of the wide 12cm of long 12cm, cleans up; Drawing the length of side is that 40nm spacing is the quadrate array figure of 20nm, and imported in the PC being connected with electron beam pattern generator, by PC, control electron beam pattern generator and this quadrate array figure is arrived to the middle of substrate by the scale of 1:1, put into baking oven with dry 30 minutes of the temperature of 60 ℃, making has the position of figure to UV transparent on substrate, forms mask plate.
(2) provide clean dry substrate, and on substrate, evenly apply positivity ultraviolet photoresist, front baking, makes the adhesive curing of positivity ultraviolet photolithographic, forms photoresist material substrate;
Select the glass substrate of the thick 0.5cm of the wide 12cm of long 12cm, use successively chromic acid scavenging solution, liquid detergent and washed with de-ionized water, then glass substrate is put into baking oven, with the temperature of 150 ℃, be dried 15 minutes; Then spin coating positivity ultraviolet photoresist (the present embodiment be GP18 series U.V. positive photoresist) on glass substrate, and by high speed rotating, make the photoresist material on glass substrate cover equably whole glass pane surface, the thickness of controlling photoresist material is 40nm; Described in inciting somebody to action, be coated with positivity ultraviolet photoresist substrate and put into baking oven, with 60 ℃ of bakings 2 hours, photoresist material is solidified, make the substrate with photoresist material.
(3) described mask plate is stacked on described photoresist material substrate, after exposing, develop, go cull post bake under ultraviolet ray, obtains the forming mould with described nanostructure graphics shape groove;
By smooth being stacked on the prepared formation photoresist material of step (2) substrate of the prepared mask plate of step (1), be then placed under UV-light exposure 15 seconds; Taking off after mask plate put into concentration with the substrate of photoresist material is that 15% developing solution soaks 60 minutes, thereby the photoresist material through ultraviolet exposure that the figure on masked plate is hidden dissolves; Photoresist material substrate after developing is placed in plasma etching machine to etching 15 minutes, remove in groove through ultraviolet exposure but do not dissolved photoresist material completely; By through going the photoresist material substrate of cull to put into baking oven, with 80 ℃ of bakings 1 hour, thereby the photoresist material of substrate is solidified, obtain the shaping dies with designed quadrate array diagram shape groove, this groove be square, the length of side is 40nm.
(4) adopt chemical synthesis metal refining in described forming mould;
Adopt chemical reduction method: the above-mentioned forming mould with quadrate array diagram shape groove is immersed in ethylene glycol solvent, with this photoresist material substrate of complete submergence, be advisable, add the AgNO that 40mL concentration is 0.2mol/L
3with 60mL concentration be 10% polyvinylpyrrolidone (PVP) solution, and add 0.5g Na
2s, controlling solution temperature is 45 ℃, stirring reaction, after 15 minutes, deposits 5 minutes, in the groove of forming mould, forms the silver nanoparticle array structure that one deck length of side is the square of 40nm.
(5) the described forming mould that has deposited metal is placed in acetone, ultrasonic depolymerization, obtains the metal Nano structure of described nanostructure figure.
It is in 20% acetone that the described forming mould that has deposited silver nanoparticle array structure is placed on to concentration, sonic oscillation 30 minutes, remove residue photoresist material and remove the Nano silver grain on photoresist material simultaneously, obtaining the length of side is the silver nanoparticle array structure (as shown in Figure 1 and Figure 2) of the square of 40nm.
The length of side that the embodiment of the present invention makes is that the silver nanoparticle array structure of the square of 40nm can be directly used in making solar cell surface antireflection structure, the accurate control of shape, size, position has improved efficiency of light absorption, and the efficiency of conversion of solar cell is improved greatly.
Embodiment bis-
A preparation method for metal Nano structure, comprises the following steps:
(1) provide clean substrate, and on substrate, make required nanostructure figure, form mask plate, on described substrate, have the position of figure to UV transparent;
Select the ferric oxide substrate of the thick 0.5cm of the wide 5cm of long 5cm, clean up rear standby; Drawing the length of side is that 30nm spacing is the quadrate array figure of 30nm, and imported in the PC being connected with Laser pattern generation system, by PC, control Laser pattern generation system and this quadrate array figure is arrived to the middle of substrate by the scale of 1:1, put into baking oven with dry 20 minutes of the temperature of 80 ℃, make mask plate.
(2) provide clean dry substrate, and on substrate, evenly apply positivity ultraviolet photoresist, front baking, makes the adhesive curing of positivity ultraviolet photolithographic, forms photoresist material substrate;
Select gallium oxide substrate and the ferric oxide substrate of the thick 0.5cm of the wide 5cm of long 5cm, use successively chromic acid scavenging solution, liquid detergent and washed with de-ionized water, then gallium oxide substrate is put into baking oven, with the temperature of 200 ℃, be dried 10 minutes; Spin coating positivity ultraviolet photoresist (the present embodiment is SUN-115P ultraviolet positive photoresist) on clean dried gallium oxide substrate, and pass through high speed rotating, make the photoresist material on gallium oxide substrate cover equably whole gallium oxide substrate surface, the thickness of controlling photoresist material is 30nm; The described substrate that is coated with positivity ultraviolet photoresist is put into baking oven, with 80 ℃ of bakings 1 hour, photoresist material is solidified, form photoresist material substrate.
(3) described mask plate is stacked on described photoresist material substrate, after exposing, develop, go cull post bake under ultraviolet ray, obtains the forming mould with described nanostructure graphics shape groove;
By smooth being stacked on the prepared formation photoresist material of step (2) substrate of the prepared mask plate of step (1), be then placed under UV-light exposure 15 seconds; Taking off after mask plate put into concentration with the substrate of photoresist material is that 20% developing solution soaks 30 minutes, thereby the photoresist material through ultraviolet exposure that the figure on masked plate is hidden dissolves; Photoresist material substrate after developing is placed in plasma etching machine to etching 15 minutes, remove in groove through ultraviolet exposure but do not dissolved photoresist material completely; By through going the photoresist material substrate of cull to put into baking oven, with 50 ℃ of bakings 2 hours, thereby the photoresist material of gallium oxide substrate is solidified, obtain the forming mould with designed quadrate array diagram shape groove, this groove be square, the length of side is 30nm.
(4) adopt chemical synthesis metal refining in described forming mould;
Adopt photoreduction met hod: the AgNO that is 0.05mol/L in 50mL concentration
3in solution, add 0.8g tri-hydration Trisodium Citrates, form mixed solution, the above-mentioned forming mould with designed quadrate array diagram shape groove is immersed in this mixed solution, the rectangular pyramid silver nanoparticle array structure blocking with the ultraviolet source induced growth of 365nm wavelength, induction time is 30 minutes, the silver nanoparticle array structure bottom surface length of side obtaining is 30nm, and height is 18nm.
(5) the described forming mould that has deposited metal is placed in acetone, ultrasonic depolymerization, obtains the metal Nano structure of described nanostructure figure.
It is in 20% acetone that the described photoresist material substrate that has deposited rectangular pyramid shape silver nanoparticle array structure is placed on to concentration, sonic oscillation 20 minutes, remove residue photoresist material and remove the Nano silver grain on photoresist material simultaneously, obtaining the bottom surface length of side is the silver nanoparticle array structure (as shown in Figure 3) of the high rectangular pyramid for 18nm of 30nm.
Embodiment tri-
A preparation method for metal Nano structure, comprises the following steps:
(1) provide clean substrate, and on substrate, make required nanostructure figure, form mask plate, on described substrate, have the position of figure to UV transparent;
Select the chromium substrate of the thick 0.3cm of the wide 2cm of long 2cm, clean up rear standby; Drawing the length of side is that 20nm spacing is the quadrate array figure of 10nm, and imported in the PC being connected with copier, by PC, control copier this quadrate array figure is duplicated to the middle of chromium substrate in the ratio of 1:2, put into baking oven with dry 20 minutes of the temperature of 80 ℃, making has the position of figure to UV transparent on substrate, forms mask plate.
(2) provide clean dry substrate, and on substrate, evenly apply positivity ultraviolet photoresist, front baking, makes the adhesive curing of positivity ultraviolet photolithographic, forms photoresist material substrate;
Select the silicon substrate of the thick 0.3cm of the wide 2cm of long 2cm, use successively chromic acid scavenging solution, liquid detergent and washed with de-ionized water, then silicon substrate is put into baking oven, with the temperature of 180 ℃, be dried 13 minutes; Spin coating positivity ultraviolet photoresist on clean dried silicon substrate (the present embodiment is for take poly-N-(p-carboxyl phenyl) the Methacrylamide ultraviolet positive photoresist that N-phenylmaleimide is main raw altogether of multipolymer), and pass through high speed rotating, make the photoresist material on glass substrate cover equably whole glass pane surface, the thickness of controlling photoresist material is 50nm; Described in inciting somebody to action, be coated with positivity ultraviolet photoresist substrate and put into baking oven, with 50 ℃ of bakings 2 hours, photoresist material is solidified, form photoresist material substrate.
(3) described mask plate is stacked on described photoresist material substrate, after exposing, develop, go cull post bake under ultraviolet ray, obtains the forming mould with described nanostructure graphics shape groove;
By the prepared mask plate of step (1) smooth be stacked in the prepared substrate with photoresist material of step (2), be then placed under UV-light exposure 15 seconds; Taking off after mask plate put into concentration with the substrate of photoresist material is that 15% developing solution soaks 60 minutes, thereby the photoresist material through ultraviolet exposure that the figure on masked plate is hidden dissolves; Photoresist material substrate after developing is placed in plasma etching machine to etching 10 minutes, remove in groove through ultraviolet exposure but do not dissolved photoresist material completely; By through going the photoresist material substrate of cull to put into baking oven, with 50 ℃ of bakings 2 hours, thereby the photoresist material of substrate is solidified, obtain the forming mould with designed quadrate array diagram shape groove, this groove rectangular parallelepiped, bottom surface is the square of length of side 40nm, cup depth is 50nm.
(4) adopt chemical synthesis metal refining in described forming mould;
Adopt irradiation method: the Al that preparation 100mL concentration is 0.1mol/L
2(SO
4)
3solution, adds 0.1g tri-hydration Trisodium Citrates, forms mixed solution; The above-mentioned forming mould with designed quadrate array diagram shape groove is put into beaker, then pour this mixed solution into, add-on, is used with standard with this photoresist material substrate of complete submergence
60the aluminium nano array structure of the rectangular pyramid that C0 gamma-ray irradiation induced growth blocks, induction time is 40 minutes, and the aluminum nanoparticles bottom surface length of side obtaining is 40nm, and height is 25nm.
(5) the described forming mould that has deposited metal is placed in acetone, ultrasonic depolymerization, obtains the metal Nano structure of described nanostructure figure.
It is in 30% acetone that the described photoresist material substrate that has deposited the aluminium nano array structure of rectangular pyramid is placed on to concentration, sonic oscillation 30 minutes, remove residue photoresist material and remove the aluminum nanoparticles on photoresist material simultaneously, obtaining the bottom surface length of side is the aluminium nano array structure of the high rectangular pyramid for 25nm of 40nm.
Embodiment tetra-
A preparation method for metal Nano structure, comprises the following steps:
(1) provide clean substrate, and on substrate, make required nanostructure figure, form mask plate, on described substrate, have the position of figure to UV transparent;
Select the ferric oxide substrate of the thick 0.3cm of the wide 1cm of long 1cm, clean clean rear air-dry standby; With X ray, at ferric oxide substrate, evenly wearing the length of side is that 30nm spacing is the square light hole of 10nm, forms mask plate.
(2) provide clean dry substrate, and on substrate, evenly apply positivity ultraviolet photoresist, front baking, makes the adhesive curing of positivity ultraviolet photolithographic, forms photoresist material substrate;
Select the glass substrate of the thick 0.3cm of the wide 1cm of long 1cm, use successively chromic acid scavenging solution, liquid detergent and washed with de-ionized water, then glass substrate is put into baking oven, with the temperature of 150 ℃, be dried 13 minutes.Spin coating positivity ultraviolet photoresist on clean dried glass substrate (the present embodiment is GP18 series U.V. positive photoresist), and pass through high speed rotating, make the photoresist material on glass substrate " get rid of " equably whole glass pane surface, the thickness of controlling photoresist material is 35nm; Described in inciting somebody to action, be coated with positivity ultraviolet photoresist substrate and put into baking oven, with 50 ℃ of bakings 2 hours, photoresist material is solidified, make the substrate with photoresist material.
(3) described mask plate is stacked on described photoresist material substrate, after exposing, develop, go cull post bake under ultraviolet ray, obtains the forming mould with described nanostructure graphics shape groove;
By the prepared mask plate of step (1) smooth be stacked in the prepared substrate with photoresist material of step (2), be then placed under UV-light exposure 12 seconds; Taking off after mask plate put into concentration with the substrate of photoresist material is that 20% developing solution soaks 30 minutes, thereby the photoresist material through ultraviolet exposure that the figure on masked plate is hidden dissolves; Photoresist material substrate after developing is placed in plasma etching machine to etching 10 minutes, remove in groove through ultraviolet exposure but do not dissolved photoresist material completely; By through going the photoresist material substrate of cull to put into baking oven, with 50 ℃ of bakings 2 hours, thereby the photoresist material of substrate is solidified, obtain the forming mould with designed rectangular parallelepiped array groove, this groove is rectangular parallelepiped, and the bottom surface length of side is 30nm, and cup depth is 35nm.
(4) adopt chemical synthesis metal refining in described forming mould;
Adopt polyvalent alcohol method: the above-mentioned photoresist material substrate with designed array of figure shape groove is immersed in ethylene glycol solution, with this photoresist material substrate of submergence just, be advisable, add the ZnSO that 30mL concentration is 0.5mol/L
3, stir and be heated to 60 ℃, react 20 minutes, start natural sediment, depositing time is 6 minutes, in groove, forming one deck bottom surface length of side is that 30nm thickness is the rectangular parallelepiped zinc nano array structure of 20nm.
(5) the described forming mould that has deposited metal is placed in acetone, ultrasonic depolymerization, obtains the metal Nano structure of described nanostructure figure.
It is in 10% acetone that the described photoresist material substrate that has deposited zinc nano array structure is placed on to concentration, sonic oscillation 60 minutes, remove residue photoresist material and remove the zinc nanoparticle on photoresist material simultaneously, obtaining the bottom surface length of side is that 30nm thickness is the rectangular parallelepiped zinc nano array structure of 20nm.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a preparation method for metal Nano structure, is characterized in that, comprises the following steps:
(1) provide clean substrate, and on substrate, make required nanostructure figure, form mask plate, on described substrate, have the position of figure to UV transparent;
(2) provide clean dry substrate, and on substrate, evenly apply positivity ultraviolet photoresist, front baking, makes the adhesive curing of positivity ultraviolet photolithographic, forms photoresist material substrate;
(3) described mask plate is stacked on described photoresist material substrate, after exposing, develop, go cull post bake under ultraviolet ray, obtains the forming mould with described nanostructure graphics shape groove;
(4) adopt chemical synthesis metal refining in described forming mould;
(5) the described forming mould that has deposited metal is immersed in acetone soln, ultrasonic depolymerization, obtains the metal Nano structure of described nanostructure figure.
2. the preparation method of a kind of metal Nano structure according to claim 1, is characterized in that, the material of the described substrate of step (1) is wolfram steel, ferric oxide or chromium.
3. the preparation method of a kind of metal Nano structure according to claim 1, it is characterized in that, the nanostructure figure that step (1) is described, adopts copier, Laser pattern generation system or electron beam pattern generator to draw, or adopts X ray to scribe.
4. the preparation method of a kind of metal Nano structure according to claim 1, is characterized in that, the described substrate of step (2) is glass substrate, silicon substrate or gallium oxide substrate.
5. the preparation method of a kind of metal Nano structure according to claim 1, is characterized in that, the substrate that step (2) is described, and its sizes and shape is identical with described mask plate.
6. the preparation method of a kind of metal Nano structure according to claim 1, it is characterized in that, the described positivity ultraviolet photoresist of step (2) is GP18 series U.V. positive photoresist, SUN-115P ultraviolet positive photoresist, or take poly-N-(p-carboxyl phenyl) Methacrylamide of the multipolymer ultraviolet positive photoresist that N-phenylmaleimide is main raw altogether.
7. the preparation method of a kind of metal Nano structure according to claim 1, is characterized in that, the described chemical synthesis of step (4) is chemical reduction method, photoreduction met hod, irradiation method or polyvalent alcohol method.
8. the preparation method of a kind of metal Nano structure according to claim 1, is characterized in that, the described metal of step (4) is silver.
9. the preparation method of a kind of metal Nano structure according to claim 1, is characterized in that, the metal Nano structure that step (5) is described, is the array structure of square, rectangular parallelepiped or rectangular pyramid.
10. the preparation method of a kind of metal Nano structure according to claim 1, is characterized in that, the metal Nano structure that step (5) is described is the array structure of the square of length of side 40nm.
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