CN101665902B - Nickel ordered porous array film and preparation method thereof - Google Patents
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Abstract
The invention discloses a nickel ordered porous array film and a preparation method thereof. The film consists of nickel ordered porous arrays, holes in the arrays are regular hexagonal or circular and are arranged in a hexagonal period, the diagonals or the diameters of the holes are 650 to 1,600 nanometers, the hole pitch is 200 to 1,000 nanometers, the hole period is 1,000 to 2,000 nanometers, the thickness of the film is 20 to 50 nanometers, and the void ratio is 60 to 90 percent. The method comprises the following steps: firstly placing polystyrene suspension on a rotary planar substrate to obtain a single-layer colloidal crystal template, then heating the template for 6 to 15 minutes at the temperature of between 60 and 150 DEG C, later placing the template in argon atmosphere and etching the template for 6 to 100 minutes by plasma, heating the template for 0 to 15 minutes at the temperature of between 60 and 150 DEG C, thermally evaporating nickel metal to the treated template at the temperature of between 900 and 1,000 DEG C under the pressure of 1-9*10<-5>Pa, and placing the template in dichloromethane solution for supersonic treatment for 5 to 120 seconds to obtain the film. The nickel ordered porous array film and the preparation method thereof can be applied in the fields of high-density magnetic storage media, sensors, invisible materials, efficient catalysts and the like.
Description
Technical field
The present invention relates to a kind of nickel film and preparation method, especially a kind of nickel ordered porous array film and preparation method thereof.
Background technology
Nickel ordered porous array film has caused people's extensive concern as the new generation of high density magnetic storage medium.Because the intrinsic anisotropy of nickel ordered porous film and the demagnetizing field of film interact, around orderly hole, form stable magnetic and raise structure, form magnetic recording unit between the adjacent hole.This nickel ordered porous array film has the advantages such as influence that Curie temperature height, magnetic recording are stablized, magnetic recording density is high and can not be subjected to superparamagnetism than magnetic nanometer separate unit array structure, in addition, nickel ordered porous array film all has potential to use at aspects such as transmitter, stealth material and effective catalysts.
At present, people are in order to obtain nickel ordered porous array film, done multiple effort, as 307～310 pages of 494 phases of solid film magazine in 2006 reported that Cheng etc. delivers be entitled as " applying nano ball lithographic method synthesis cycle nickel silicide nanometer lattice row " (S.L.Cheng et al., Fabrication ofperiodic nickel silicide nanodot arrays using nanosphere lithography, The solid films 494 (2006): article 307-310), after this article discloses a kind of suspension manufacturing of using polystyrene and has the individual layer lamina membranacea in high-sequential zone, synthesize the method that obtains the nickel silicide nanometer lattice row by the method for evaporation thereon again.But, no matter be synthetic method, or its finished product, all exist weak point, at first, the preparation of polystyrene colloid monolayer crystal masterplate is more numerous and diverse, needs to use the suspension of organic surface active agent SDS (Sodium Dodecylsulfate) p-poly-phenyl ethene to dilute earlier according to specific ratio, and then be placed in the humidistat under ultransonic condition, solvent evaporation to be fallen, obtain polystyrene colloid monolayer crystal masterplate just now; Secondly, because the polystyrene colloid ball on the colloid monolayer crystal masterplate that makes is together tightly packed, so, the evaporation nickel that carries out thereon subsequently, and remove the technology of polystyrene colloid monolayer crystal masterplate and the synthetic nickel silicide nanometer lattice row that obtains is a kind of dot matrix of being made up of the isolated trilateral nano particle of nickel, be not connected with each other between nano particle wherein and particle and form film, restricted the performance and the wide application field of the excellence that is had when it uses as film.
Summary of the invention
The technical problem to be solved in the present invention is for overcoming weak point of the prior art, provides between a kind of Kong Yukong of ordered porous array to be the nickel ordered porous array film of nano level nickel film.
Another technical problem that the present invention will solve is for providing a kind of preparation method of nickel ordered porous array film.
For solving technical problem of the present invention, the technical scheme that is adopted is: nickel ordered porous array film comprises nickel ordered porous array, particularly described nickel ordered porous array is film like, hole in the described film is regular hexagon or circle, and be six side's periodic arrangement, the diagonal lines in described hole or diameter are that 650～1600nm, pitch of holes are that 200～1000nm, hole cycle are 1000～2000nm; The thickness of described film is that 20～50nm, voidage are 60～90%.
For solving another technical problem of the present invention, another technical scheme that is adopted is: the preparation method of nickel ordered porous array film comprises polystyrene suspension, and particularly completing steps is as follows:
Step 1, the polystyrene suspension that with the colloidal spheres diameter is 1000～2000nm earlier places on the planar substrates of rotation, obtain closelypacked colloid monolayer crystal template, colloid monolayer crystal template being placed temperature is 60～150 ℃ of heating 6～15min down again, afterwards, be placed on earlier and use plasma etching 6～100min under the argon atmospher, being placed on temperature again is 60～150 ℃ of heating 0～15min down;
Step 2, will place pressure through the colloid monolayer crystal template that step 1 was handled earlier is 1～9 * 10
-5Pa, temperature are 900～1000 ℃ of hot evaporation metal nickel 3～9h down, are placed on supersound process 5～120s in the dichloromethane solution again, make nickel ordered porous array film.
As the preparation method's of nickel ordered porous array film further improvement, the speed of rotation of described planar substrates is 50～80r/min; Described is 60～150 ℃ down before heating 6～15min colloid monolayer crystal template being placed temperature, earlier it is immersed in the water, after treating that it breaks away from substrate and swim on the water surface, with the substrate of required material and shape it is picked up, and make it be covered in substrate surface; Described water is deionized water or distilled water; Described substrate is conductor or semi-conductor or isolator; Described substrate be shaped as plane or convex-shaped or concave shape; Described etching power during with plasma etching is 6～18W; The purity of described metallic nickel is 〉=99.9%; Described dichloromethane solution is an analytical reagent, and its content is 〉=99.5%; Frequency of ultrasonic during described supersound process is that 30～50KHz, power are 90～110W.
Beneficial effect with respect to prior art is, one, use field emission scanning electron microscope and specific surface and voidage analyser to carry out the sign of form and specific surface area respectively to intermediate product and the film that makes respectively, from the stereoscan photograph that obtains with nitrogen adsorption-the desorption graphic representation as can be known, intermediate product is the colloid monolayer crystal template that orderly many ball array constitute, globe in the template independently exists separately, and it is keeping spacing each other, is non-close-packed structure.Film is made of nickel ordered porous array, hole in the array is regular hexagon or circle, and be six side's periodic arrangement, the diagonal lines in hole or diameter are that 650～1600nm, pitch of holes are that 200～1000nm, hole cycle are 1000～2000nm, and the thickness of film is that 20～50nm, voidage are 60～90%; They are two years old, use superconducting quantum interference device (SQUID) to carry out the sign of magnetic property to the film that makes, from the magnetic hysteresis loop figure that obtains as can be known, compare with the fine and close nickel film of atresia that the same terms prepares down, the coercive force of film and remanent magnetism all have increase, and after its annealing, its coercive force also significantly increases, promptly, can regulate effectively the magnetic of film by the aperture in the orderly hole of control; They are three years old, preparation method's science, feasible and effective, neither need organic surface active agent, the product that makes is again a film, also can reasonably control the size of hole by the time of control plasma etching, form the nickel ordered porous array film in different apertures, and prepare the nickel ordered porous array film in different hole cycle by the polystyrene suspension of selecting different spherical diameter, more can carry out thermal deformation and handle, the pattern of hole is taken place by regular hexagon to circular controllable variations by the colloid monolayer crystal template of the non-dense set packed structures after the article on plasma body etching.Simultaneously, the preparation method is the synthetic nickel ordered porous array film of big area at low cost, makes it be suitable for large-scale industrial production and is easy to business-like applying.
Further embodiment as beneficial effect, the one, the speed of rotation of planar substrates is preferably 50～80r/min, except that the formation of having guaranteed colloid monolayer crystal template, also the colloidal spheres in the polystyrene suspension can not thrown away planar substrates and cause unnecessary waste; The 2nd, be 60～150 ℃ down before heating 6～15min colloid monolayer crystal template being placed temperature, earlier it is immersed in the water, after treating its disengaging substrate and swimming on the water surface, substrate with required material and shape picks up it, and make it be covered in substrate surface, can with film preparation on the substrate of required material and shape, greatly increase the suitability of film; The 3rd, the etching power during with plasma etching is preferably 6～18W, and the frequency of ultrasonic during supersound process is preferably 30～50KHz, power is preferably 90～110W, all can guarantee the quality of film better.
Description of drawings
Below in conjunction with accompanying drawing optimal way of the present invention is described in further detail.
Fig. 1 is the SEM photo that uses Japanese JEOL6700 type field emission scanning electron microscope (SEM) to observe the back take to the intermediate product that makes.Can be found out that by the SEM photo intermediate product is the colloid monolayer crystal template that orderly many ball array constitute, the ball in the template is non-close-packed structure.
Fig. 2 is the SEM photo that uses Japanese JEOL6700 type field emission scanning electron microscope (SEM) to observe the back take to the film that makes.Can be found out that by the SEM photo the orderly hole in the film is a circular port, its bore dia is 650nm, and the hole cycle is 1000nm.
Fig. 3 is the SEM photo that uses Japanese JEOL6700 type field emission scanning electron microscope (SEM) to observe the back take to the film that makes.Can be found out that by the SEM photo the orderly hole in the film is a circular port, its bore dia is 1600nm, and the hole cycle is 2000nm.
Fig. 4 is in preparation process, and the colloid monolayer crystal template after the article on plasma body etching does not carry out that thermal deformation is handled and SEM photo that the film that makes uses Japanese JEOL6700 type field emission scanning electron microscope (SEM) to observe the back take.Can be found out that by the SEM photo the orderly hole in the film is a regular hexagon, its diagonal lines is 1600nm, and the hole cycle is 2000nm.
Fig. 5 is to be that the fine and close nickel film of atresia of 20nm and the film that makes use superconducting quantum interference device (SQUID) to carry out the magnetic hysteresis loop figure that obtains after magnetic property is measured to thickness respectively; X-coordinate among the figure is that magneticstrength, ordinate zou are squareness ratio, and the magnetic field that adds during measurement is parallel to the face direction of film.S0 among the figure is the magnetic hysteresis loop of the fine and close nickel film of atresia; S1, S2 and S3 are the magnetic hysteresis loop of circular port film, wherein, thickness with film of S1, S2 and S3 magnetic hysteresis loop is 20nm, the hole cycle is 1000nm in order, bore dia with film of S1 magnetic hysteresis loop is 800nm, bore dia with film of S2 magnetic hysteresis loop is 650nm, and the membrane pores diameter with S3 magnetic hysteresis loop is 900nm.
Fig. 6 uses superconducting quantum interference device (SQUID) to carry out the magnetic hysteresis loop figure that obtains after magnetic property is measured after placing 300 ℃ of following nitrogen atmosphere annealing 200min to the film that makes with the film that makes respectively; X-coordinate among the figure is that magneticstrength, ordinate zou are squareness ratio, and the magnetic field that adds during measurement is parallel to the face direction of film.S4 among the figure and S5 are the magnetic hysteresis loop of the orderly hole of regular hexagon film, wherein, thickness with film of S4 and S5 magnetic hysteresis loop is 20nm, the hole cycle is 2000nm in order, hole diagonal lines with film of S4 magnetic hysteresis loop is 1600nm, film with S5 magnetic hysteresis loop is the film after annealing, and its hole diagonal lines is 1600nm.
Embodiment
At first make with ordinary method or buy the polystyrene suspension that the colloidal spheres diameter is 1000～2000nm from market, material is conductor, semi-conductor and isolator, is shaped as the substrate of plane, convex-shaped and concave shape, the metallic nickel of purity 〉=99.9%.Then,
Embodiment 1
The concrete steps of preparation are: step 1, the polystyrene suspension that with the colloidal spheres diameter is 1000nm earlier places on the planar substrates of rotation, obtain closelypacked colloid monolayer crystal template, again colloid monolayer crystal template is immersed in the water, after treating its disengaging substrate and swimming on the water surface, substrate with required material and shape picks up it, and makes it be covered in substrate surface, and being placed on temperature then is 60 ℃ of heating 15min down; Wherein, the speed of rotation of planar substrates is 50r/min, and water is deionized water, and substrate is plane isolator.Afterwards, be placed on earlier and use plasma etching 6min under the argon atmospher, being placed on temperature again is 60 ℃ of heating 15min down; Wherein, the etching power during with plasma etching is 18W, obtains the colloid monolayer crystal template that non-dense set is as shown in Figure 1 piled up.
Step 2, will place pressure through the colloid monolayer crystal template that step 1 was handled earlier is 1 * 10
-5Pa, temperature are 900 ℃ of hot evaporation metal nickel 9h down, are placed on supersound process 5s in the dichloromethane solution again; Wherein, the purity of metallic nickel is 99.9%, and dichloromethane solution is the analytical reagent of content 99.9%, and the ultrasonic frequency during supersound process is that 30KHz, power are 110W.Make as shown in Figure 2, and the nickel ordered porous array film shown in the S2 magnetic hysteresis loop in having Fig. 5.
Embodiment 2
The concrete steps of preparation are: step 1, the polystyrene suspension that with the colloidal spheres diameter is 1250nm earlier places on the planar substrates of rotation, obtain closelypacked colloid monolayer crystal template, again colloid monolayer crystal template is immersed in the water, after treating its disengaging substrate and swimming on the water surface, substrate with required material and shape picks up it, and makes it be covered in substrate surface, and being placed on temperature then is 80 ℃ of heating 13min down; Wherein, the speed of rotation of planar substrates is 60r/min, and water is deionized water, and substrate is plane isolator.Afterwards, be placed on earlier and use plasma etching 25min under the argon atmospher, being placed on temperature again is 80 ℃ of heating 13min down; Wherein, the etching power during with plasma etching is 15W, obtains being similar to the colloid monolayer crystal template that non-dense set shown in Figure 1 is piled up.
Step 2, will place pressure through the colloid monolayer crystal template that step 1 was handled earlier is 3 * 10
-5Pa, temperature are 930 ℃ of hot evaporation metal nickel 7.5h down, are placed on supersound process 30s in the dichloromethane solution again; Wherein, the purity of metallic nickel is 99.99%, and dichloromethane solution is the analytical reagent of content 99.8%, and the ultrasonic frequency during supersound process is that 35KHz, power are 105W.Make be similar to shown in Figure 2, and the nickel ordered porous array film shown in the S1 magnetic hysteresis loop in having Fig. 5.
The concrete steps of preparation are: step 1, the polystyrene suspension that with the colloidal spheres diameter is 1500nm earlier places on the planar substrates of rotation, obtain closelypacked colloid monolayer crystal template, again colloid monolayer crystal template is immersed in the water, after treating its disengaging substrate and swimming on the water surface, substrate with required material and shape picks up it, and makes it be covered in substrate surface, and being placed on temperature then is 100 ℃ of heating 10min down; Wherein, the speed of rotation of planar substrates is 65r/min, and water is deionized water, and substrate is plane isolator.Afterwards, be placed on earlier and use plasma etching 50min under the argon atmospher, being placed on temperature again is 100 ℃ of heating 8min down; Wherein, the etching power during with plasma etching is 12W, obtains being similar to the colloid monolayer crystal template that non-dense set shown in Figure 1 is piled up.
Step 2, will place pressure through the colloid monolayer crystal template that step 1 was handled earlier is 5 * 10
-5Pa, temperature are 950 ℃ of hot evaporation metal nickel 6h down, are placed on supersound process 60s in the dichloromethane solution again; Wherein, the purity of metallic nickel is 99.9%, and dichloromethane solution is the analytical reagent of content 99.7%, and the ultrasonic frequency during supersound process is that 40KHz, power are 100W.Make be similar to shown in Figure 3, and the nickel ordered porous array film shown in the S3 magnetic hysteresis loop in having Fig. 5.
Embodiment 4
The concrete steps of preparation are: step 1, the polystyrene suspension that with the colloidal spheres diameter is 1750nm earlier places on the planar substrates of rotation, obtain closelypacked colloid monolayer crystal template, again colloid monolayer crystal template is immersed in the water, after treating its disengaging substrate and swimming on the water surface, substrate with required material and shape picks up it, and makes it be covered in substrate surface, and being placed on temperature then is 130 ℃ of heating 8min down; Wherein, the speed of rotation of planar substrates is 70r/min, and water is deionized water, and substrate is plane isolator.Afterwards, be placed on earlier and use plasma etching 75min under the argon atmospher, being placed on temperature again is 130 ℃ of heating 4min down; Wherein, the etching power during with plasma etching is 9W, obtains being similar to the colloid monolayer crystal template that non-dense set shown in Figure 1 is piled up.
Step 2, will place pressure through the colloid monolayer crystal template that step 1 was handled earlier is 7 * 10
-5Pa, temperature are 980 ℃ of hot evaporation metal nickel 4.5h down, are placed on supersound process 90s in the dichloromethane solution again; Wherein, the purity of metallic nickel is 99.99%, and dichloromethane solution is the analytical reagent of content 99.6%, and the ultrasonic frequency during supersound process is that 45KHz, power are 95W.Make and be similar to shown in Figure 3ly, and be similar to the nickel ordered porous array film shown in the S3 magnetic hysteresis loop that has among Fig. 5.
Embodiment 5
The concrete steps of preparation are: step 1, the polystyrene suspension that with the colloidal spheres diameter is 2000nm earlier places on the planar substrates of rotation, obtain closelypacked colloid monolayer crystal template, again colloid monolayer crystal template is immersed in the water, after treating its disengaging substrate and swimming on the water surface, substrate with required material and shape picks up it, and makes it be covered in substrate surface, and being placed on temperature then is 150 ℃ of heating 6min down; Wherein, the speed of rotation of planar substrates is 80r/min, and water is deionized water, and substrate is plane isolator.Afterwards, be placed on earlier and use plasma etching 100min under the argon atmospher, being placed on temperature again is 150 ℃ of heating 0min down; Wherein, the etching power during with plasma etching is 6W, obtains being similar to the colloid monolayer crystal template that non-dense set shown in Figure 1 is piled up.
Step 2, will place pressure through the colloid monolayer crystal template that step 1 was handled earlier is 9 * 10
-5Pa, temperature are 1000 ℃ of hot evaporation metal nickel 3h down, are placed on supersound process 120s in the dichloromethane solution again; Wherein, the purity of metallic nickel is 99.9%, and dichloromethane solution is the analytical reagent of content 99.5%, and the ultrasonic frequency during supersound process is that 50KHz, power are 90W.Make as shown in Figure 4, and the nickel ordered porous array film shown in the S4 magnetic hysteresis loop in having Fig. 6.
Selecting material more respectively for use is conductor or semi-conductor or isolator, be shaped as substrate plane or convex-shaped or concave shape, repeat the foregoing description 1～5, same as or be similar to Fig. 2 or Fig. 3 or shown in Figure 4, and as or be similar to the S1 that has among Fig. 5 or the nickel ordered porous array film shown in the S4 magnetic hysteresis loop among S2 or S3 or Fig. 6.
Obviously, those skilled in the art can carry out various changes and modification to nickel ordered porous array film of the present invention and preparation method thereof and not break away from the spirit and scope of the present invention.Like this, if of the present invention these are revised and modification belongs within the scope of claim of the present invention and equivalent technologies thereof, then the present invention also is intended to comprise these changes and modification interior.
Claims (10)
1. a nickel ordered porous array film comprises nickel ordered porous array, it is characterized in that:
Described nickel ordered porous array is film like, and the hole in the described film is regular hexagon or circle, and is six side's periodic arrangement, and the diagonal lines in described hole or diameter are that 650～1600nm, pitch of holes are that 200～1000nm, hole cycle are 1000～2000nm;
The thickness of described film is that 20～50nm, voidage are 60～90%.
2. the preparation method of the described nickel ordered porous array film of claim 1 comprises polystyrene suspension, it is characterized in that completing steps is as follows:
Step 1, the polystyrene suspension that with the colloidal spheres diameter is 1000～2000nm earlier places on the planar substrates of rotation, obtain closelypacked colloid monolayer crystal template, colloid monolayer crystal template being placed temperature is 60～150 ℃ of heating 6～15min down again, afterwards, be placed on earlier and use plasma etching 6～100min under the argon atmospher, being placed on temperature again is 60～150 ℃ of heating 0～15min down;
Step 2, will place pressure through the colloid monolayer crystal template that step 1 was handled earlier is 1～9 * 10
-5Pa, temperature are 900～1000 ℃ of hot evaporation metal nickel 3～9h down, are placed on supersound process 5～120s in the dichloromethane solution again, make nickel ordered porous array film.
3. the preparation method of nickel ordered porous array film according to claim 2, the speed of rotation that it is characterized in that planar substrates is 50～80r/min.
4. the preparation method of nickel ordered porous array film according to claim 2, it is characterized in that colloid monolayer crystal template being placed temperature be 60～150 ℃ down before heating 6～15min, earlier it is immersed in the water, after treating its disengaging substrate and swimming on the water surface, substrate with required material and shape picks up it, and makes it be covered in substrate surface.
5. the preparation method of nickel ordered porous array film according to claim 4 is characterized in that substrate is a conductor, or semi-conductor, or isolator.
6. the preparation method of nickel ordered porous array film according to claim 5 is characterized in that being shaped as of substrate is plane, or convex-shaped, or concave shape.
7. the preparation method of nickel ordered porous array film according to claim 2, the etching power when it is characterized in that with plasma etching is 6～18W.
8. the preparation method of nickel ordered porous array film according to claim 2, the purity that it is characterized in that metallic nickel is 〉=99.9%.
9. the preparation method of nickel ordered porous array film according to claim 2 is characterized in that dichloromethane solution is an analytical reagent, and its content is 〉=99.5%.
10. the preparation method of nickel ordered porous array film according to claim 2, the frequency of ultrasonic when it is characterized in that supersound process is that 30～50KHz, power are 90～110W.
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| CN102050419B (en) * | 2010-12-02 | 2012-08-15 | 台州学院 | Magnetic double nano-structure array material and preparation method thereof |
| CN102383102B (en) * | 2011-09-29 | 2013-10-16 | 中国航空工业集团公司北京航空材料研究院 | Magnetic nano anti-dot array film and preparation method thereof |
| CN103194740B (en) * | 2012-01-10 | 2015-04-29 | 中国科学院合肥物质科学研究院 | Preparation method of metal silver ordered porous array membrane |
| CN103529081B (en) * | 2013-10-21 | 2016-02-03 | 苏州慧闻纳米科技有限公司 | A kind of preparation method of multiple layer metal oxide porous membrane gas-sensitive nano material |
| CN105350077B (en) * | 2015-10-20 | 2018-06-26 | 同济大学 | A kind of method that photonic crystal scintillator is prepared using polymer template |
| CN108018531B (en) * | 2017-11-27 | 2020-04-17 | 天津大学 | Method for preparing nano porous metal material |
| CN108538617A (en) * | 2018-04-02 | 2018-09-14 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of three-dimensional ordered polyporous material |
| CN110441986B (en) * | 2019-08-01 | 2022-09-06 | 肇庆市华师大光电产业研究院 | Preparation method of nano microsphere photoetching template |
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| CN1555072A (en) * | 2003-12-21 | 2004-12-15 | 浙江大学 | Method for producing nano magnetic network structure film |
| CN1962951A (en) * | 2006-11-30 | 2007-05-16 | 复旦大学 | Method for preparing c-shaft vertically aligned L10 phase FePt magnetic recording film |
| CN101110453A (en) * | 2007-04-26 | 2008-01-23 | 复旦大学 | Process for producing TiO*/metallic array electrode with ordered nano-structure |
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| CN1555072A (en) * | 2003-12-21 | 2004-12-15 | 浙江大学 | Method for producing nano magnetic network structure film |
| CN1962951A (en) * | 2006-11-30 | 2007-05-16 | 复旦大学 | Method for preparing c-shaft vertically aligned L10 phase FePt magnetic recording film |
| CN101110453A (en) * | 2007-04-26 | 2008-01-23 | 复旦大学 | Process for producing TiO*/metallic array electrode with ordered nano-structure |
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