CN104141108A - Method for manufacturing size-controllable two-dimensional nanostructure of CrN nanopore array - Google Patents
Method for manufacturing size-controllable two-dimensional nanostructure of CrN nanopore array Download PDFInfo
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Abstract
The invention discloses a method for manufacturing a size-controllable two-dimensional nanostructure of a CrN nanopore array. The method for manufacturing the size-controllable two-dimensional nanostructure of the CrN nanopore array comprises the following steps that (1) a substrate is placed in a mixed solution of ammonia water and hydrogen peroxide, and then hydrophilia treatment is conducted by means of ultrasonic waves; (2) a single-layer template on which macromolecular nanoballs are arranged periodically is manufactured on the substrate according to a rotary coating method; (3) the macromolecular nanoballs are etched with oxygen as the etching treatment gas, and then a new single-layer template is obtained after etching; (4) CrN sputtering deposition are conducted on the single-layer template obtained after etching in the step (3) through a closed field non-equilibrium magnetron sputtering ion plating system; (5) the template obtained after deposition in the step (4) is placed in organic solvent, and then the macromolecular nanoballs are dissolved away. According to the method for manufacturing the size-controllable two-dimensional nanostructure of the CrN nanopore array, an array template is manufactured by combining the nanoball rotary-coating technology and the nanoball photoetching method, and the array temperature with the size precision accurately controllable can be manufactured by adjusting the technological conditions.
Description
Technical field
The invention belongs to technical field of material, be specifically related to a kind of method of two-dimensional nanostructure controlled dimensions of CrN nanohole array.
Background technology
In recent years, the research of periodic nano-structure array has been obtained more and more widely paying attention to, several technology that can manufacturing cycle nano-structure array comprise chemical etching, X ray engraving method, el (EBL) and molecular beam epitaxy (MBE) etc.Although etching technique can be controlled the form of these arrays, its expensive and complicated process has limited its application.Therefore, many researchists attempt developing low-cost, high-throughput, high-resolution etching technique.
Nano imprint lithography (NIL) is as a kind of alternative method, has low cost and the simple advantage of preparation, can produce large-scale nanostructure, and different times that can copying nano structure.
In the preparation process of solid-ceramic coating, need to use closed field unbalanced magnetron sputtering ion plating system to carry out the deposition of film, make solid-ceramic coating there are excellent frictional property, thermostability, antistick and anticorrosion properties.
Nanometer ball photoetching technique (NSL) is a kind of technology for the manufacture of nano die array, has low cost and the simple advantage of preparation, is also a kind of method of high yield.
But, in currently available technology, also exist many deficiencies, the problem that comprises anti-adhesion effectiveness (high contact angle and low surface free energy) prepared by nano die has to be solved, and therefore, developing new low surface free energy coated material has become and put forward high performance key.
Summary of the invention
For deficiency of the prior art, the invention provides a kind of method of two-dimensional nanostructure controlled dimensions of CrN nanohole array, the method adopts nanometer ball to revolve the accurately controlled array mould plate of approach preparation size precision that cloth technology and nanometer ball photoetching technique (NSL) combine, then rely on this template to utilize closed field unbalanced magnetron sputtering ion plating system (closed field unbalanced magnetron sputtering ion plating system, CFUBMIP) carry out the deposition of CrN film, form nano-pore array structure.
The present invention is achieved through the following technical solutions: a kind of method of two-dimensional nanostructure controlled dimensions of CrN nanohole array, and the method comprises the following steps: (1) is placed in substrate the mixing solutions of ammoniacal liquor and hydrogen peroxide, ultrasonicly carries out wetting ability processing; (2) by the single tier templates of the method for spin coating macromolecule nanometer ball that preparation cycle is arranged on substrate; (3) use oxygen as etch processes gas, macromolecule nanometer ball is carried out to etching, obtain the single tier templates after etching; (4) by closed field unbalanced magnetron sputtering ion plating system, the single tier templates after to the etching in step (3) is carried out the sputtering sedimentation of CrN; (5) post-depositional template in step (4) is placed in to organic solvent, dissolves and remove macromolecule nanometer ball.
The present invention adopts nanometer ball to revolve the approach that cloth technology and nanometer ball photoetching combine to prepare array mould plate, by the adjustment to processing condition, can prepare accurately controlled array mould plate of dimensional precision.
As preferably, in described step (1), in the mixing solutions of ammoniacal liquor and hydrogen peroxide, the volume ratio of ammoniacal liquor and hydrogen peroxide is 1:1.The object of wetting ability processing is to create a hydrophilic surface on substrate.
As preferably, in described step (2), the rotating speed of rotary coating machine is 1200 rpm, rotation time 4 minutes.Under this condition, can obtain the much the same nanometer ball array of diameter.
As preferably, in described step (3), the power of etch processes is 50w, and the time is 10 ~ 35 minutes, by controlling etching period, can obtain the macromolecule nanometer ball that size is different, and under the same time, the size of the macromolecule nanometer ball obtaining is similar.
As preferably, in described step (4), in the sputter deposition process of CrN, the distance between template and target is 150 mm, and the pressure of foundation of sputter cavity is evacuated to 1.5 × 10
-5torr, substrate bias is-70V, Cr target current 1A, and utilize spectral emissions monitor regulate nitrogen flow and control Coating composition.
The present invention utilizes closed field unbalanced magnetron sputtering ion plating system to carry out the deposition of CrN film, be deposited in the space between macromolecule nanometer ball, acquisition has the single tier templates of CrN-macromolecule nanometer ball package structure, these processing condition can ensure that CrN has good deposition effect simultaneously, the nanostructure forming has the feature of low surface free energy, and there is excellent burnish resistance, thermostability, antistick and anticorrosion properties.
As preferably, in described step (5), dissolve the process of removing macromolecule nanometer ball and divide and carry out for three times, wherein organic solvent is methylene dichloride for the first time, and organic solvent is acetone for the second time, and organic solvent is ethanol for the third time.Select three kinds of water-soluble organic solutions from small to large, can well dissolve macromolecule nanometer ball, leave the nano-pore structure of CrN, this nano-pore array structure has an orderly two-dimensionally periodic structure.
As preferably, described macromolecule nanometer ball material therefor is the one in polymethylmethacrylate, polyethylene, polypropylene, polyvinyl chloride, polystyrene.
Compared with prior art, the present invention has following beneficial effect: the present invention realizes the macromolecule nanometer ball single tier templates that creates the periodic arrangement of self-assembly by rotary coating machine on substrate, obtains the CrN nanohole array of an orderly two-dimensionally periodic structure.
CrN nanohole array prepared by the present invention has low surface free energy.
Preparation technology of the present invention, equipment are simple, with low cost, and controllability is strong, and technological process has very high repeatability, and nano-pore array structure productive rate is higher, and prepared nano-pore array structure any surface finish is not polluted.
The method that the present invention prepares two-dimensional nano hole array structure has certain universality, the nanometer ball that utilizes in theory different size on substrate is single tier templates, recycling nanometer ball photoetching technique is carried out the size regulation and control of nanometer ball, can obtain the nanostructure of the nanohole array with different size size.
Brief description of the drawings
Fig. 1 is step 1,2 schematic diagram that the present invention prepares CrN nanohole array.
Fig. 2 is step 3,4,5 schematic diagram that the present invention prepares CrN nanohole array.
Fig. 3 is flat scanning Electronic Speculum of the present invention (SEM) figure.
Wherein, (a) be flat scanning Electronic Speculum (SEM) figure of the single tier templates of periodic arrangement polystyrene (PS) nanometer ball of self-assembly 540 nm of the present invention.(b) figure of the flat scanning Electronic Speculum (SEM) after to PS nanometer ball size attenuate (etching power 50W, times 20 min) via etching (RIE) technique.
Fig. 4 is flat scanning Electronic Speculum (SEM) figure and the statistical graph of CrN nanohole array of the present invention.
Wherein, figure (a) and (b), (c) and (d) be the CrN two-dimensional nanostructure of the different size to PS nanometer ball size attenuate via RIE technique, etching power is 50W, etching period is respectively 10 min, 20 min, 25 min, 35 min; Figure (e), (f) are the graph of a relation of size and the spacing etching period of nanoporous in different samples.
Fig. 5 is atomic force microscope figure and the CrN nanohole array depth error figure of sample of the present invention.
Wherein, the RIE processing parameter of this sample is power 50W, etching period 10 min, and two-dimentional pattern and the depth section of the image of demonstration and corresponding line sweep, show that the degree of depth of nanoporous is about 100 ± 5 nm.
Fig. 6 is the graph of a relation between diameter and the surface free energy of CrN nanohole array.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1 comprises the following steps: it is 1:1 ammoniacal liquor (NH that silicon substrate is immersed into volume ratio by (1)
4and hydrogen peroxide (H OH)
2o
2) in mixing solutions, carry out ultrasonic cleaning 30 minutes, then use deionized water wash 10 minutes.
(2) taking polystyrene (PS) as macromolecule raw material, utilize rotary coating machine to be rotated coating, setting speed 1200 rpm, carry out 4 min, after stopping, can obtaining polystyrene (PS) the nanometer ball single tier templates of the periodic arrangement of self-assembly as shown in Fig. 3 (a).
(3) by reactive ion etching, the nanometer ball in single tier templates is carried out to size regulation and control, power parameter is set as 50W, and etching period is 10min, uses oxygen as etch processes gas, obtains the polystyrene nanospheres single tier templates after size regulation and control.
(4) then use closed field unbalanced magnetron sputtering ion plating system (CFUBMIP), the silicon substrate template of polystyrene (PS) nanometer ball of adjusting size is contained in cavity, carry out the sputtering sedimentation of CrN film, the pressure of foundation of sputter cavity is evacuated to 1.5 × 10
-5torr, the argon flow amount of setting is 25 sccm, be set as-70V of substrate bias, Cr target current 1A, distance between base material and target is set as 150 mm, utilizes spectral emissions monitor (Optical Emission Monitor, OEM) to regulate nitrogen flow simultaneously, to maintain that target surface sputtering hits and sedimentation state dynamically constant, thereby accurately control Coating composition.
(5) after the deposition of CrN film finishes, base material is immersed at methylene dichloride (CH
2cl
2) carrying out ultrasonic washing 10 minutes in solution, methylene dichloride dissolved polystyrene nanometer ball is to remove this polystyrene nanospheres single tier templates; Then utilize acetone (CH
3cOCH
3) ultrasonic cleaning 5 minutes; Finally at ethanol (C
2h
5oH) ultrasonic cleaning 5 minutes.Thus obtained CrN nano-pore array structure has an orderly two-dimensionally periodic structure, and calculate surface free energy by using three kinds of test(ing) liquids to measure: distilled water (distilled water), ethylene glycol (ethylene glycol) and methylene iodide (diiodomethane).
Fig. 4 (a) is flat scanning Electronic Speculum (SEM) figure of the CrN nano-pore array structure of 540 nm, and the diameter that can be measured nanoporous by figure is 347 ± 9 nm, and the height of CrN nanohole array is 100 ± 5 nm.The surface free energy calculating is 43.52 MN/M, as shown in Figure 6.
Embodiment 2 comprises the following steps: it is 1:1 ammoniacal liquor (NH that silicon substrate is immersed into volume ratio by (1)
4and hydrogen peroxide (H OH)
2o
2) in mixing solutions, carry out ultrasonic cleaning 30 minutes, then use deionized water wash 10 minutes.
(2) taking polystyrene (PS) as macromolecule raw material, utilize rotary coating machine to be rotated coating, setting speed 1200 rpm, carry out 4 min, after stopping, can obtaining polystyrene (PS) the nanometer ball single tier templates of the periodic arrangement of self-assembly as shown in Fig. 3 (a).
(3) by reactive ion etching, the nanometer ball in single tier templates is carried out to size regulation and control, power parameter is set as 50W, etching period 20min, uses oxygen as etch processes gas, as Fig. 3 (b) is depicted as the polystyrene nanospheres single tier templates after size regulation and control.
(4) then use closed field unbalanced magnetron sputtering ion plating system (CFUBMIP), the silicon substrate template of polystyrene (PS) nanometer ball of adjusting size is contained in cavity, carry out the sputtering sedimentation of CrN film, the pressure of foundation of sputter cavity is evacuated to 1.5 × 10
-5torr, the argon flow amount of setting is 25 sccm, be set as-70V of substrate bias, Cr target current 1A, distance between base material and target is set as 150 mm, utilizes spectral emissions monitor (Optical Emission Monitor, OEM) to regulate nitrogen flow simultaneously, to maintain that target surface sputtering hits and sedimentation state dynamically constant, thereby accurately control Coating composition.
(5) after the deposition of CrN film finishes, base material is immersed at methylene dichloride (CH
2cl
2) carrying out ultrasonic washing 10 minutes in solution, methylene dichloride dissolved polystyrene nanometer ball is to remove this polystyrene nanospheres single tier templates; Then utilize acetone (CH
3cOCH
3) ultrasonic cleaning 5 minutes; Finally at ethanol (C
2h
5oH) ultrasonic cleaning 5 minutes.Thus obtained CrN nano-pore array structure has an orderly two-dimensionally periodic structure, and calculate surface free energy by using three kinds of test(ing) liquids to measure: distilled water (distilled water), ethylene glycol (ethylene glycol) and methylene iodide (diiodomethane).
Fig. 4 (b) is flat scanning Electronic Speculum (SEM) figure of the CrN nano-pore array structure of 540 nm, and the diameter that can be measured nanoporous by figure is 266 ± 11nm, and the height of CrN nanohole array is 100 ± 5 nm.The surface free energy calculating is 38.24 MN/M, as shown in Figure 6.
Embodiment 3 comprises the following steps: it is 1:1 ammoniacal liquor (NH that silicon substrate is immersed into volume ratio by (1)
4and hydrogen peroxide (H OH)
2o
2) in mixing solutions, carry out ultrasonic cleaning 30 minutes, then use deionized water wash 10 minutes.
(2) taking polystyrene (PS) as macromolecule raw material, utilize rotary coating machine to be rotated coating, setting speed 1200 rpm, carry out 4 min, after stopping, can obtaining polystyrene (PS) the nanometer ball single tier templates of the periodic arrangement of self-assembly as shown in Fig. 3 (a).
(3) by reactive ion etching, the nanometer ball in single tier templates is carried out to size regulation and control, power parameter is set as 50W, and etching period 25min uses oxygen as etch processes gas, obtains the polystyrene nanospheres single tier templates after size regulation and control.
(4) then use closed field unbalanced magnetron sputtering ion plating system (CFUBMIP), the silicon substrate template of polystyrene (PS) nanometer ball of adjusting size is contained in cavity, carry out the sputtering sedimentation of CrN film, the pressure of foundation of sputter cavity is evacuated to 1.5 × 10
-5torr, the argon flow amount of setting is 25 sccm, be set as-70V of substrate bias, Cr target current 1A, distance between base material and target is set as 150 mm, utilizes spectral emissions monitor (Optical Emission Monitor, OEM) to regulate nitrogen flow simultaneously, to maintain that target surface sputtering hits and sedimentation state dynamically constant, thereby accurately control Coating composition.
(5) after the deposition of CrN film finishes, base material is immersed at methylene dichloride (CH
2cl
2) carrying out ultrasonic washing 10 minutes in solution, methylene dichloride dissolved polystyrene nanometer ball is to remove this polystyrene nanospheres single tier templates; Then utilize acetone (CH
3cOCH
3) ultrasonic cleaning 5 minutes; Finally at ethanol (C
2h
5oH) ultrasonic cleaning 5 minutes.Thus obtained CrN nano-pore array structure has an orderly two-dimensionally periodic structure, and calculate surface free energy by using three kinds of test(ing) liquids to measure: distilled water (distilled water), ethylene glycol (ethylene glycol) and methylene iodide (diiodomethane).
Fig. 4 (c) is flat scanning Electronic Speculum (SEM) figure of the CrN nano-pore array structure of 540 nm, and the diameter that can be measured nanoporous by figure is 228 ± 11 nm, and the height of CrN nanohole array is 100 ± 5 nm.The surface free energy calculating is 34.85 MN/M, as shown in Figure 6.
Embodiment 4 comprises the following steps: it is 1:1 ammoniacal liquor (NH that silicon substrate is immersed into volume ratio by (1)
4and hydrogen peroxide (H OH)
2o
2) in mixing solutions, carry out ultrasonic cleaning 30 minutes, then use deionized water wash 10 minutes.
(2) taking polystyrene (PS) as macromolecule raw material, utilize rotary coating machine to be rotated coating, setting speed 1200 rpm, carry out 4 min, after stopping, can obtaining polystyrene (PS) the nanometer ball single tier templates of the periodic arrangement of self-assembly as shown in Fig. 3 (a).
(3) by reactive ion etching, the nanometer ball in single tier templates is carried out to size regulation and control, power parameter is set as 50W, and etching period 35min uses oxygen as etch processes gas, obtains the polystyrene nanospheres single tier templates after size regulation and control.
(4) then use closed field unbalanced magnetron sputtering ion plating system (CFUBMIP), the silicon substrate template of polystyrene (PS) nanometer ball of adjusting size is contained in cavity, carry out the sputtering sedimentation of CrN film, the pressure of foundation of sputter cavity is evacuated to 1.5 × 10
-5torr, the argon flow amount of setting is 25 sccm, be set as-70V of substrate bias, Cr target current 1A, distance between base material and target is set as 150 mm, utilizes spectral emissions monitor (Optical Emission Monitor, OEM) to regulate nitrogen flow simultaneously, to maintain that target surface sputtering hits and sedimentation state dynamically constant, thereby accurately control Coating composition.
(5) after the deposition of CrN film finishes, base material is immersed at methylene dichloride (CH
2cl
2) carrying out ultrasonic washing 10 minutes in solution, methylene dichloride dissolved polystyrene nanometer ball is to remove this polystyrene nanospheres single tier templates; Then utilize acetone (CH
3cOCH
3) ultrasonic cleaning 5 minutes; Finally at ethanol (C
2h
5oH) ultrasonic cleaning 5 minutes.Thus obtained CrN nano-pore array structure has an orderly two-dimensionally periodic structure, and calculate surface free energy by using three kinds of test(ing) liquids to measure: distilled water (distilled water), ethylene glycol (ethylene glycol) and methylene iodide (diiodomethane).
Fig. 4 (d) is flat scanning Electronic Speculum (SEM) figure of the CrN nano-pore array structure of 540 nm, and the diameter that can be measured nanoporous by figure is 166 ± 12 nm, and the height of CrN nanohole array is 100 ± 5 nm.The surface free energy calculating is 26.75 MN/M, as shown in Figure 6.
Fig. 5 has shown the relation between nanoporous diameter and surface free energy.Surface free energy is linear because the reduction that contact angle can improve nanoporous roughness with the increase of nanoporous diameter.Therefore, surface free energy reducing and present lower surface free energy with nanoporous diameter.
In the present invention, being used to form macromolecule nanometer ball material therefor can also be the one in polymethylmethacrylate, polyethylene, polypropylene, polyvinyl chloride.
Above elected as preferred embodiment of the present invention, not in order to limit the present invention, all any amendments of doing within the spirit and principles in the present invention, be equal to replace and improve, within being all included in protection scope of the present invention.
Claims (7)
1. a method for the two-dimensional nanostructure controlled dimensions of CrN nanohole array, the method comprises the following steps: (1) is placed in substrate the mixing solutions of ammoniacal liquor and hydrogen peroxide, ultrasonicly carries out wetting ability processing; (2) by the single tier templates of the method for spin coating macromolecule nanometer ball that preparation cycle is arranged on substrate; (3) use oxygen as etch processes gas, macromolecule nanometer ball is carried out to etching, obtain the single tier templates after etching; (4) by closed field unbalanced magnetron sputtering ion plating system, the single tier templates after to the etching in step (3) is carried out the sputtering sedimentation of CrN; (5) post-depositional template in step (4) is placed in to organic solvent, dissolves and remove macromolecule nanometer ball.
2. the method for the two-dimensional nanostructure controlled dimensions of a kind of CrN nanohole array according to claim 1, is characterized in that, in the mixing solutions of the middle ammoniacal liquor of described step (1) and hydrogen peroxide, the volume ratio of ammoniacal liquor and hydrogen peroxide is 1:1.
3. the method for the two-dimensional nanostructure controlled dimensions of a kind of CrN nanohole array according to claim 2, is characterized in that, in described step (2), the rotating speed of rotary coating machine is 1200 rpm, rotation time 4 minutes.
4. the method for the two-dimensional nanostructure controlled dimensions of a kind of CrN nanohole array according to claim 3, is characterized in that, in described step (3), the power of etch processes is 50w, and the time is 10 ~ 35 minutes.
5. the method for the two-dimensional nanostructure controlled dimensions of a kind of CrN nanohole array according to claim 4, it is characterized in that, in described step (4), in the sputter deposition process of CrN, the distance between template and target is 150 mm, and the pressure of foundation of sputter cavity is evacuated to 1.5 × 10
-5torr, substrate bias is-70V, Cr target current 1A, and utilize spectral emissions monitor regulate nitrogen flow and control Coating composition.
6. the method for the two-dimensional nanostructure controlled dimensions of a kind of CrN nanohole array according to claim 5, it is characterized in that, dissolving the process of removing macromolecule nanometer ball in described step (5) divides and carries out for three times, wherein organic solvent is methylene dichloride for the first time, organic solvent is acetone for the second time, and organic solvent is ethanol for the third time.
7. according to a kind of method that improves the controlled light extraction efficiency of metal nano pore structure described in claim 1 to 6 any one, it is characterized in that, described macromolecule nanometer ball material therefor is the one in polymethylmethacrylate, polyethylene, polypropylene, polyvinyl chloride, polystyrene.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152128A (en) * | 2015-09-22 | 2015-12-16 | 宁波工程学院 | Method for forming Cr two-dimensional hole type nanoring array structure with controllable size |
| CN111186813A (en) * | 2020-01-14 | 2020-05-22 | 江苏师范大学 | Composite nanopore array substrate based on microsphere self-assembly and inclined angle deposition technology and preparation method thereof |
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| CN1887688A (en) * | 2006-07-14 | 2007-01-03 | 清华大学 | Prepn process of nanometer dot array in controllable size with inverse porous nanometer ball template |
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2014
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| CN1887688A (en) * | 2006-07-14 | 2007-01-03 | 清华大学 | Prepn process of nanometer dot array in controllable size with inverse porous nanometer ball template |
Non-Patent Citations (1)
| Title |
|---|
| HUNG-CHUNWU等: "Fabrication of size-tunable antireflective nanopillar array using hybrid nano-patterning lithography", 《SURFACE & COATINGS TECHNOLOGY》, vol. 240, 15 February 2014 (2014-02-15), pages 413 - 418, XP028829970, DOI: doi:10.1016/j.surfcoat.2013.12.066 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105152128A (en) * | 2015-09-22 | 2015-12-16 | 宁波工程学院 | Method for forming Cr two-dimensional hole type nanoring array structure with controllable size |
| CN111186813A (en) * | 2020-01-14 | 2020-05-22 | 江苏师范大学 | Composite nanopore array substrate based on microsphere self-assembly and inclined angle deposition technology and preparation method thereof |
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