CN102169819B - Method of preparing nanometer metal structure - Google Patents
Method of preparing nanometer metal structure Download PDFInfo
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- CN102169819B CN102169819B CN 201110008475 CN201110008475A CN102169819B CN 102169819 B CN102169819 B CN 102169819B CN 201110008475 CN201110008475 CN 201110008475 CN 201110008475 A CN201110008475 A CN 201110008475A CN 102169819 B CN102169819 B CN 102169819B
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Abstract
The invention discloses a method of preparing nanometer metal structure, relating to the metal nanometer technology. By realizing an etched structure with a certain depth to width ratio on a silicon surface, nanometer metal lines discrete with each other can be realized, thereby expanding the application scope of the conventional method; and by utilizing a high-temperature contact and a low-temperature peel-off, the success rate and reliability of the technology are improved substantially, which is more propitious to the actual application. By the method, the manufacture success rate of sample is improved, nanometer metal structure of high-precision and ultra-smooth can be realized in various substrates, and the defect of conventional metal sediment peel-off method is overcome. Therefore, a preparation method of high performance, precision and being capable of realizing the nanometer metal structure of discrete structure is provided.
Description
Technical field
The present invention relates to a kind of method for preparing nanometer metal structure, particularly the meticulous lithographic technique of the high-aspect-ratio of silicon materials is combined with metal deposition technique, the preparation metal Nano structure.
Background technology
The electron density that forms under Electromagnetic Field based on the metal surface rises and falls---the correlative study of surface phasmon, and launch gradually in the application in a plurality of fields such as detection, sensing, photoelectricity be integrated.But the fine silicon materials process technology with respect to maturation, at present people also can not satisfy the needs of phasmon technical development far away to the machining accuracy of metal material, all are difficult to realization such as the metallic pattern processing of nanoscale and the metal Nano structure of super-smooth surface.Under this background, people have proposed a kind of new metal structure process technology---metal deposition stripping method, has the silicon materials surface deposition metal of ad hoc structure, utilize the relatively poor characteristic of metal and silicon face adhesive force, metal structure with silicon face is stripped to the other materials surface again, " can be applicable to the ultra-smooth metallic pattern of phasmon device and super material " (Ultrasmooth Patterned Metals for Plasmonicsand Metamaterials) such as document one, be stated from " Science ", 2009, Vol.325:594 is disclosed.But deposition lift-off technology before can only be realized the structure of all-metal material, namely can only form fluctuating or the fold of metal surface, can not form the metal wire that is separated from each other, and discrete metal structure is then needed in the phasmon technology practice often.In addition, the mode of directly the peeling off success rate that traditional metal deposition stripping means adopts is lower, and repeatability can not be satisfactory.
Summary of the invention
The objective of the invention is to disclose a kind of method for preparing nanometer metal structure, can overcome the defective of early stage metal deposition stripping means, efficiently, accurately realize the nanometer metal structure of separate structure.Simultaneously, improve the power that is made into of sample, can realize in various types of substrates the nanometer metal structure of fine, ultra-smooth.
For achieving the above object, technical solution of the present invention is:
A kind of method for preparing nanometer metal structure, it comprises step:
1) get smooth, a smooth silicon chip, the nano graph that utilizes mask etching or focused ion etching that the silicon chip upper surface is formed to have certain depth-to-width ratio is clean with its surface clean and use drying nitrogen to dry up again;
2) in step 1) in the sample surfaces deposit metallic material that makes, be formed with the metal level of graphic structure;
3) get smooth, a smooth substrate, have the glue-line of certain viscosity at the even spin coating one deck of substrate upper surface;
4) with step 2) in gained sample upset, make metal level tip upside down on step 3 downwards) in gained the substrate upper surface of glue-line is arranged, with metal level and glue-line close contact;
5) again to step 4) the gained sample toasts, and makes its rapid cooling after the end to be baked again; Make metal level and glue-line close attachment by expanding with heat and contract with cold;
6) to step 5) treated sample, carrying out silicon chip peels off, with step 1) described in silicon chip and step 2) described in metal level separate, make metal level transfer to step 3) described in the substrate glue-line on, thereby form the nanometer metal structure of fine, ultra-smooth.
The described method for preparing nanometer metal structure, its described silicon chip, or the surface is the multilayered material sheets of silicon layer, is silicon-on-insulator (SOI, silicon on insulator), smooth cleaning will be processed through polishing and ultrasonic cleaning in its surface.
The described method for preparing nanometer metal structure, its described step 1) the certain depth-to-width ratio in, refer to: maximum line width is not more than 1: 3 with the ratio of etching depth in the silicon materials surfacial pattern; Surface clean is to process with ultrasonic cleaning.
The described method for preparing nanometer metal structure, its described step 2) metal material in is the metal material lower with silicon chip adhesive force, is gold, silver, copper one of them or alloy; The thickness of deposit metallic material is no more than 1/3 of silicon materials etching depth.
The described method for preparing nanometer metal structure, its described step 3) substrate in, for silicon chip, titanium dioxide silicon chip, glass, quartz, sapphire, gallium nitride material sheet one of them, substrate is processed smooth cleaning through surface finish and ultrasonic cleaning.
The described method for preparing nanometer metal structure, its described step 3) glue-line in, for SU8 glue, PMMA glue, HSQ glue, polyamides vinyl material one of them, the adhesive force of this glue-line and deposit metallic material is greater than the adhesive force of silicon and deposit metallic material.
The described method for preparing nanometer metal structure, its described step 5) baking in is to adopt hot plate or baking oven to carry out, and baking temperature and stoving time determine according to glue line material character; Rapidly cooling is the sample after the baking to be inserted low temperature refrigerator or the mode that contacts with cold temperature source realizes that cooling extent and time are determined by use glue line material thermal coefficient of expansion.
The described method for preparing nanometer metal structure, its described cold temperature source is alcohol, water, ice cube, dry ice, liquid nitrogen, helium one of them or combination.
The advantage of the inventive method is:
By realize the etching structure of certain depth-to-width ratio at silicon face, can realize mutually discrete nano metal lines, thereby expand the range of application of conventional deposition stripping means; In addition, utilize the method that high temperature contacts and low temperature is peeled off, greatly improved success rate and the reliability of technique, more be conducive to practical application.
Description of drawings
Fig. 1 is a kind of method flow diagram for preparing nanometer metal structure of the present invention;
Fig. 2 is a kind of procedure schematic diagram for preparing nanometer metal structure of the present invention; Wherein:
Fig. 2 a is 1 in the inventive method) the step schematic diagram;
Fig. 2 b is 2 in the inventive method) the step schematic diagram;
Fig. 2 c is 3 in the inventive method) the step schematic diagram;
Fig. 2 d is 3 in the inventive method) the step schematic diagram;
Fig. 2 e is 4 in the inventive method) the step schematic diagram;
Fig. 2 f is 6 in the inventive method) the step schematic diagram.
The drawing explanation:
The smooth silicon chip that 1 expression has the nanostructure of certain depth-to-width ratio;
The metal level of 2 expression depositions;
Smooth, the smooth substrate of 3 expressions;
4 expressions have the glue-line of certain viscosity.
Embodiment
A kind of method for preparing nanometer metal structure of the present invention may further comprise the steps:
1) on smooth, smooth silicon chip, the nano graph that utilizes mask etching or focused ion etching that silicon chip surface is formed to have certain depth-to-width ratio, its surface clean is clean and use drying nitrogen to dry up again, shown in Fig. 2 a.
Silicon chip comprises that also the surface is the multilayered material sheets of silicon layer (such as silicon-on-insulator (SOI)), requires its surface to process smooth cleaning through polishing and ultrasonic cleaning.
Certain depth-to-width ratio in the method refers to: maximum line width is not more than 1: 3 with the ratio of etching depth in the silicon materials surfacial pattern.
2) in step 1) in the sample surfaces deposit metallic material that makes, be formed with the metal level of graphic structure, shown in Fig. 2 b.Deposit metallic material comprises the metal materials lower with silicon chip adhesive force such as gold, silver, copper, requires deposit metallic material thickness to be no more than 1/3 of silicon materials etching depth.
3) get smooth, a smooth substrate, shown in Fig. 2 c, have the glue-line of certain viscosity at the even spin coating one deck of substrate upper surface, shown in Fig. 2 d.Substrate comprises the various types of materials sheets such as silicon chip, titanium dioxide silicon chip, glass, quartz, sapphire, gallium nitride, requires substrate to process smooth cleaning through surface finish and ultrasonic cleaning.
Glue-line can be selected according to actual needs, such as materials such as SU8 glue, PMMA glue, HSQ glue, polyamides vinyls.
Certain viscosity of glue-line refers to that the adhesive force of this glue-line of requirement and deposit metallic material is greater than the adhesive force of silicon and deposit metallic material.
4) with step 2) in the sample upset that makes, make metal level tip upside down on step 3 downwards) in make the substrate upper surface of glue-line, make step 2) described in metal level and step 3) described in the glue-line close contact, shown in Fig. 2 e.
5) to step 4) sample of gained toasts, and makes its rapid cooling after the end to be baked again; Make step 2 by expanding with heat and contract with cold) described in metal level and step 3) described in the glue-line close attachment.Baking can adopt hot plate or baking oven to carry out, and baking temperature and stoving time determine according to glue line material character.Rapidly temperature-fall period can by insert low temperature refrigerator or with contact cold temperature source (such as alcohol, water, ice cube, dry ice, liquid nitrogen, helium) mode and realize that cooling extent is determined by use glue line material thermal coefficient of expansion.
6) to step 5) treated sample, carrying out silicon chip peels off, with step 1) described in silicon chip and step 2) described in metal level separate, make metal level transfer to step 3) described in the substrate glue-line on, shown in Fig. 2 f, thus the nanometer metal structure of formation fine, ultra-smooth.
Below in conjunction with embodiment and accompanying drawing the method that the present invention prepares metal Nano structure is described in detail.
Embodiment 1:
1) on smooth, smooth silicon chip, utilize electron beam exposure to form nano graph at the PMMA mask, nanometer etching technics by induction coupled reaction ion etching system carves nanostructure at silicon chip surface, its figure maximum line width is 50nm, etching depth 220nm, depth-to-width ratio is 1: 4.4; Utilize acetone, alcohol, water ultrasonic cleaning to fall the cull on surface, use drying nitrogen that silicon chip surface is dried up;
2) in step 1) in the silicon chip surface deposition 20nm gold (Au) that makes, be formed with gold (Au) metal level of structure;
3) even spin coating one deck SU8 glue on smooth, smooth quartz plate;
4) with step 2) in the sample upset that makes, tip upside down on step 3) in the sample surfaces that makes, make step 2) described in gold (Au) metal level and step 3) described in SU8 glue-line close contact;
5) utilizing hot plate to through step 4) sample processed toasts, and baking temperature is 155 degrees centigrade, stoving time 30 minutes; End to be baked was inserted sample in 0 degree centigrade the refrigerator ten minutes; Make step 2 by expanding with heat and contract with cold) described in Au metal level and step 3) described in SU8 glue-line close attachment;
6) from through step 5) on the sample processed, with step 1) described in silicon chip peel off, make step 2) described in gold (Au) metal level transfer to step 3) described on the substrate SU8 glue-line, thereby form the nanometer metal structure of fine, ultra-smooth at the SU8 glue-line.
Embodiment 2:
The preparation method of present embodiment is roughly identical with embodiment 1, and just condition is as described below:
Utilize the focused-ion-beam lithography method directly to form the nanostructure figure at smooth, smooth silicon chip surface, its figure maximum line width is 30nm, etching depth 120nm, and depth-to-width ratio is 1: 4; After cleaning dries up, at its surface deposition 25nm silver (Ag); Even spin coating one deck polyimide resin on smooth, smooth gallium nitride substrate subsequently, to have silver nanostructured silicon chip tips upside down on the gallium nitride substrate that has applied polyimide resin, and utilize baking oven 130 degrees centigrade of lower bakings 1 hour, being placed on subsequently subzero 15 degrees centigrade ice cube lowered the temperature upper 15 minute, at last silicon chip is peeled away from sample, the argent nanostructure is transferred on the polyimide resin layer.
Claims (10)
1. a method for preparing nanometer metal structure is characterized in that, comprises step:
1) get a silicon chip, the nano graph that utilizes mask etching or focused ion etching that the silicon chip upper surface is formed to have certain depth-to-width ratio is clean with its surface clean and use drying nitrogen to dry up again;
2) in step 1) in the sample surfaces deposit metallic material that makes, be formed with the metal level of graphic structure;
3) get a substrate, have the glue-line of certain viscosity at the even spin coating one deck of substrate upper surface;
4) with step 2) in gained sample upset, make metal level tip upside down on step 3 downwards) in gained the substrate upper surface of glue-line is arranged, with metal level and glue-line close contact;
5) again to step 4) the gained sample toasts, and makes its rapid cooling after the end to be baked again; Make metal level and glue-line close attachment by expanding with heat and contract with cold;
6) to step 5) treated sample, carry out silicon chip and peel off, with step 1) described in silicon chip and step 2) described in metal level separate, make metal level transfer to step 3) described in the substrate glue-line on, thereby form nanometer metal structure.
2. by the method for preparing nanometer metal structure claimed in claim 1, it is characterized in that described silicon chip is that the surface is the multilayered material sheets of silicon layer, its surface will be processed through polishing and ultrasonic cleaning.
3. by the method for preparing nanometer metal structure claimed in claim 2, it is characterized in that described surface is that the multilayered material sheets of silicon layer is silicon-on-insulator.
4. by the method for preparing nanometer metal structure claimed in claim 1, it is characterized in that described step 1) in certain depth-to-width ratio, refer to: maximum line width is not more than 1: 3 with the ratio of etching depth in the silicon materials surfacial pattern; Surface clean is to process with ultrasonic cleaning.
5. by the method for preparing nanometer metal structure claimed in claim 1, it is characterized in that described step 2) in metal material, be the metal material lower with silicon chip adhesive force, be gold, silver, copper one of them or alloy; The thickness of deposit metallic material is no more than 1/3 of silicon materials etching depth.
6. by the method for preparing nanometer metal structure claimed in claim 1, it is characterized in that described step 3) in substrate, for silicon chip, titanium dioxide silicon chip, quartz, sapphire, gallium nitride material sheet one of them, substrate is processed smooth cleaning through surface finish and ultrasonic cleaning.
7. by the method for preparing nanometer metal structure claimed in claim 1, it is characterized in that described step 3) in substrate, be glass, substrate is processed smooth cleaning through surface finish and ultrasonic cleaning.
8. by the method for preparing nanometer metal structure claimed in claim 1, it is characterized in that, described step 3) glue-line in, for SU8 glue, PMMA glue, HSQ glue, polyamides vinyl material one of them, the adhesive force of this glue-line and deposit metallic material is greater than the adhesive force of silicon and deposit metallic material.
9. by the method for preparing nanometer metal structure claimed in claim 1, it is characterized in that described step 5) in baking, be to adopt hot plate or baking oven to carry out, baking temperature and stoving time determine according to glue line material character; Rapidly cooling is the sample after the baking to be inserted low temperature refrigerator or the mode that contacts with cold temperature source realizes that cooling extent and time are determined by use glue line material thermal coefficient of expansion.
10. by the method for preparing nanometer metal structure claimed in claim 9, it is characterized in that described cold temperature source is alcohol, water, ice cube, dry ice, liquid nitrogen, helium one of them or combination.
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| CN103863999B (en) * | 2012-12-13 | 2015-10-28 | 中国科学院物理研究所 | A kind of preparation method of metal Nano structure |
| CN104485279A (en) * | 2014-12-11 | 2015-04-01 | 国家纳米科学中心 | Transparent electrode based on metal nanometer grid and preparing method of transparent electrode |
| CN105070352B (en) * | 2015-07-22 | 2017-10-20 | 西安交通大学 | A kind of flexible super flat transparent conductive film and preparation method thereof |
| CN106611638A (en) * | 2016-12-30 | 2017-05-03 | 华中科技大学 | Low temperature conductive micrometer and/or nanowire network transfer method |
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| CN101580224A (en) * | 2009-06-01 | 2009-11-18 | 南京大学 | Patterning preparation method for nano array |
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| 杨海方、徐鹏、唐令、李俊杰、夏钶、顾长志.基于铁磁金属纳米点接触结构的全金属逻辑电路.《物理》.2008,第37卷(第10期),692-696. * |
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