CN102020241A - Method for realizing surface induction self-assembly of nano particles on edge of masking film - Google Patents
Method for realizing surface induction self-assembly of nano particles on edge of masking film Download PDFInfo
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- CN102020241A CN102020241A CN2010105392896A CN201010539289A CN102020241A CN 102020241 A CN102020241 A CN 102020241A CN 2010105392896 A CN2010105392896 A CN 2010105392896A CN 201010539289 A CN201010539289 A CN 201010539289A CN 102020241 A CN102020241 A CN 102020241A
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Abstract
The invention belongs to the technical field of nano structure preparation, in particular to a method for assembling nano particles by constructing a polyelectrolyte layer on a specific locus (a edge of a masking film) and utilizing adsorption property of the polyelectrolyte, namely a method for realizing surface induction self-assembling on a specific locus (an edge of a masking film). The method comprises the following steps: preparing a template, depositing the polyelectrolyte layer on the surface of the template, adding the masking film, removing the template, carrying out self-assembling on the edge of the masking film and the like. By utilizing the method for assembling on the specific locus provided by the invention, the difficulty of placing nano particles on certain microstructural edges is solved. The method provided by the invention is beneficial supplement for the existing micron and nanometer processing technique which takes a photoecctching technique and a press-printing technique as a main part, and ensures that the nano particles can be embroidered on microstructures, thus enriching the functions of the microstructures, and having the potential application in preparation of miniaturized and microminiaturized devices.
Description
Technical field
The invention belongs to the nanostructured preparing technical field, being particularly related to a kind of at specific site---polyelectrolyte layer is constructed by the edge of mask, and the characterization of adsorption that utilizes these polyelectrolyte carries out the method for nano particle assembling, promptly at specific site---and the edge of mask realizes the method for spatial induction self assembly.
Background technology
Nanometer technology is meant the ways and means of making new material, research new technology on nanoscale, producing new unit.Nanometer technology is as an emerging cross discipline, will provide a brand-new technology interface for the development of information science, life science, molecular biology, ecological science and the material science of 21 century.
Self assembly is a kind of a kind of technology by the spontaneous formation ordered structure of basic structural unit (molecule, nano material etc.).Self-assembling technique is widely used in the preparation of nano material and constructing of nano-device, is a kind of important method in nano science field.Wherein, the development of polyelectrolyte static alternating deposit technology is especially noticeable.This technology has been used to prepare the nanostructured ultrathin membrane with multiple functions such as luminous, anticorrosion, hydrophobic, sensings.By combining, can prepare the periodic structure of polyelectrolyte assembling film with mould plate technique (impression, photoetching etc.).But the development of technology needs improved preparation method day by day, need be accurate to sub-micron and nanometer to miniaturization and microminiaturized requirement, and accurately the assemble method of location (specific site) is needed development badly.
The technology close with the present invention is disclosed Chinese patent on August 6 " self-assembled structures " in 2003, publication number CN1434765.It discloses with a kind of self-assembled structures on the island of separating.These structures can be used as the integrated products device.The method of producing these products comprises positioning step and the self assembly step in the border of definition that defines device boundaries.Difference of the present invention is: be not in the assembling of the border " interior " of definition, but directly assemble on " edge " that specific process is constructed.What border " interior " defined is a two dimensional surface, and " edge " that the present invention constructs then is the one dimension linear structure.Patent different from the past the present invention proposes a kind of novel package technique based on the edge, solves at the edge or the method for boundary assembling.
Summary of the invention
The purpose of this invention is to provide a kind of method of carrying out the nano particle assembling, thereby be deposited on the problem at structural edge place with solving the nano particle location in mask edge.
(a) on substrate, be fixed for the template of constructing micrometre or nanostructured;
(b) carry out the deposition of polyelectrolyte layer on template, polyelectrolyte is PDDA[poly (diallydimethylammonium chloride), Chinese: polydiene propyl-dimethyl ammonium chlorine], thickness is 0.5～1.5 nanometer;
(c) the fixing mask on the surface of polyelectrolyte layer, the particle diameter of mask nano particle is 10～100 nanometers, mask thicknesses is suitable with the mask nano particle diameter;
(d) remove the template of introducing by in the step (a), at substrate surface, originally there was the zone of template to expose out, originally there was not the zone of template then to keep the double-decker of polyelectrolyte and mask nano particle, simultaneously expose polyelectrolyte layer, thereby obtain the alternately periodic structure of arrangement of double-decker and exposed substrate surface in mask edge;
(e) on the polyelectrolyte layer that mask edge exposes, assemble and the different types of nano particle of mask nano particle by electrostatic interaction, thereby induce self assembly in edge's realization nanoparticle surface of mask.
Said substrate can be quartz plate, silicon chip, sheet glass and macromolecule (general-purpose plastics such as polyethylene, polypropylene, polybutene, polystyrene resins, acrylic resin, phenolic resins, amino resins for example in the said method; Engineering plastics such as polyamide, Merlon and rubber) substrate, cleaning surfaces is handled the back and is used; Said template is meant the material that is used for constructing micrometre or nanostructured used in the nanoprocessing process, and the cycle of template can be from 100 nanometers～100 micron, can be micro-sphere structures, also can be list structures.It is 50 nanometers～1 millimeter that template is fixed on behind the substrate surface thickness.The periodic structure of template shows that the exposed part of substrate surface and template cover part periodically alternately occur.Template can be organic material or inorganic material, for example polystyrene colloid microballoon, PDMS (dimethyl silicone polymer, can be used for preparing the list structure template), silicon dioxide colloid microballoon etc., template is fixed on is meant on the substrate with physics spin coating method or Chemical Crosslinking Methods template be fixed on the substrate; The said polyelectrolyte deposition of carrying out on template is meant by chemical action power (Coulomb force, hydrogen bond, coordinate bond) or physical force (Van der Waals force) and makes the polyelectrolyte compound be adsorbed onto the surface of substrate and template, thickness 0.5～1.5 nanometer of polyelectrolyte layer (if assemble by multilayer with the polyelectrolyte molecules of other kind, thickness can reach 0.5～50 nanometer); Said fixedly mask is meant one deck organic material nano particle (comprising polymethylacrylic acid, poly-to vinylbenzenesulfonic acid etc.) or inorganic material nano particle (is comprised noble metal nano particles, as gold, silver, copper etc., and semi-conductor nano particles, as CdTe, CdS, ZnO, Fe
2O
3, Fe
3O
4Deng) cover substrate surface and template surface by physics or chemisorption; Said method of removing template comprises chemical attack and physical etchings, chemical attack is meant with chemical reagent (as chloroform) dissolves template or reacts that (the chloroform molecule can penetrate mask layer, erode mould material, mask layer on the template is along with the elimination of mould material comes off thereupon), physical etchings is meant utilizes plasma technology etc. that template is eliminated; Said static self assembly is meant the electrostatic attraction of the material (polyelectrolyte and nano particle) based on oppositely charged and as the assemble method of driving force.Step (e) said on the polyelectrolyte layer that mask edge exposes the assembling with the different types of nano particle of mask nano particle be organic material nano particle or inorganic material nano particle, the organic material nano particle is a polymethylacrylic acid or poly-to vinylbenzenesulfonic acid, and the inorganic material nano particle is gold, silver, copper, CdTe, CdS, ZnO, Fe
2O
3Or Fe
3O
4
On the experimental procedure basis, further can utilize the method for chemical attack or physical etchings to remove mask in the above, only stay the assembly of nano particle along mask edge.
The present invention proposes a kind of method of assembling, can solve some place nano particle at the microstructured edge place difficulty in specific site.The present invention is favourable replenishing to present little, nanofabrication technique based on photoetching technique and stamping technique, can on micro-structural, come fringing with nano particle, thereby enrich the function of micro-structural, miniaturization and microminiaturized preparation of devices are had potential application.
Description of drawings
Fig. 1: process schematic diagram of inducing self assembly in edge's realization nanoparticle surface of mask of the present invention; Wherein, step (a) is fixed cycle property list structure template on substrate, and template is wide to be 10 microns, and the template cycle is 20 microns; Step (b) is at substrate and template surface absorption polyelectrolyte compound, and thickness is 1.5 nanometers; Step (c) is in the surface coverage golden nanometer particle mask of polyelectrolyte compound layer, mask thicknesses 17 nanometers; Step (d) utilizes the method for chemical attack or physical etchings that mould material is removed, after removing mould material, originally lose attached to the material on the template and come off after depending on thing thereupon, the polyelectrolyte layer and the golden nanometer particle mask on it that directly are adsorbed on substrate surface then are retained; Step (e) is utilized the exposed polyelectrolyte absorption Nano silver grain of mask edge; Step (f) chemical attack or physical etchings method are removed mask material.
Fig. 2: embodiment 1 is described to be that template, golden nanometer particle (average diameter is 17 nanometers) are that mask, PDDA are polyelectrolyte, process schematic diagram that Nano silver grain (average diameter is 45 nanometers) is assembled in mask edge with polystyrene microsphere (diameter is 600 nanometers) individual layer ordered structure;
The each several part name is called: the polystyrene microsphere template 1 on the glass substrate, PDDA polyelectrolyte 2 in the template surface covering, golden nanometer particle mask 3 in the polyelectrolyte surface coverage, the double-decker of polyelectrolyte and mask and exposed substrate surface alternately arrange 4, at golden nanometer particle mask edge assembling Nano silver grain 5; The same Fig. 1 of each step.
The stereoscan photograph of the important sample of Fig. 3: embodiment 1 and AFM picture; A and B are respectively among the embodiment 1 shown in Figure 21 and the stereoscan photograph of 3 samples, A is that diameter is the stereoscan photograph of the polystyrene microsphere individual layer ordered structure template of 600 nanometers, the stereoscan photograph of the template of B has been surface coverage PDDA polyelectrolyte film and golden nanometer particle (average diameter 17 nanometers) mask, wherein the light spot on the ball is a golden nanometer particle; C and D are respectively the AFM picture of the structure that shown in Figure 24 and 5 samples obtain among the embodiment 1, C is exposed substrate surface (border circular areas, diameter 325 nanometers) and double-decker surface (polyelectrolyte film and mask) AFM picture of structure arranged alternately, C the picture left above is the AFM perpendicular plan view, the C top right plot is an AFM miter angle vertical view, dark border circular areas is exposed substrate surface among this two figure, light areas is the double-decker cover part, C figure below is the depth of section analysis chart of AFM, clearly shown alternately structure arranged of exposed substrate surface and double-decker surface, D is the AFM picture at double-decker (polyelectrolyte film and mask) edge absorption Nano silver grain (average diameter 45 nanometers), three figure are identical with the characterizing method of three figure among the C among the D, the most shallow spot (being positioned at border circular areas edge) of color is a Nano silver grain in D the picture left above and D top right plot, and the spike of D figure below curve has partly been represented the depth of section of Nano silver grain.
The stereoscan photograph of the sample that step among Fig. 4: the embodiment 2 (f) obtains;
The specific embodiment
Embodiment 1:
With 600 nano pipe/polyhenylethylene microballoons is that template, 17 nm of gold nano particles are that mask, PDDA are that polyelectrolyte, 45 Nano Silver nano particles are the assembling process of assembled material.
(a) (method of liquid-vaqor interface assembling referring to document: Chem.Res.Chinese U.2007 for the method for employing liquid-vaqor interface assembling, 23,712-714. microballoon is arranged as two-dimentional hexagonal closs packing structure, a similar leg-of-mutton space is arranged between three balls) fixedly polystyrene microsphere template (but polystyrene microsphere business procurement on glass substrate, average diameter 600 nanometers), form individual layer ordered structure (polystyrene microsphere two dimension hexagonal closs packing single layer structure);
(b) deposition PDDA polyelectrolyte on the surface texture of the sample of step (a) preparation, itself has positive charge PDDA, is the deposition that can finish PDDA in 0.5% the PDDA aqueous solution by the mass fraction that the sample of step (a) preparation is directly soaked;
(c) golden nanometer particle mask (golden nanometer particle average diameter 17 nanometers of on the surface texture of the sample that step (b) prepares, assembling, synthetic method is referring to document: Nature Phys.Sci.1973,241,20-22. synthetic back solution directly uses, need not to handle), the surface of golden nanometer particle own has negative electrical charge, can directly be adsorbed onto the PDDA molecular surface, and method is that the sample of step (b) preparation directly was immersed in the synthetic solution of gold nanoparticles 6 hours;
(d) remove the polystyrene colloid microsphere template of introducing in the sample for preparing by step (c), adopt method ultrasonic 1 minute in chloroform;
(e) utilize that the exposed polyelectrolyte in mask border or edge carries out the assembling of nano particle in the sample of step (d) preparation, assembled material be Nano silver grain (Nano silver grain average diameter 45 nanometers, synthetic method is referring to document: J.Phys.Chem.1982,86,3391-3395. synthetic back solution directly uses, need not to handle), Nano silver grain itself is electronegative, method is that the sample of step (d) preparation directly was immersed in the synthetic silver nano-particle solution 45 minutes, thereby is implemented in the assembling that mask edge carries out nano particle.
Embodiment 2:
With 600 nano pipe/polyhenylethylene microballoons is that template, 19 Nano Silver nano particles are that mask, PDDA are that polyelectrolyte, 17 nm of gold nano particles are the assembling process of assembled material.
As (a)～(e) step operation of embodiment 1, different is that employing 19 Nano Silver nano particles are mask in the step (c); Adopting 17 nm of gold nano particles in the step (e) is assembled material; In addition, embodiment 2 is than embodiment more than 1 one steps (f), and is as follows:
(f) sample of step (e) preparation was soaked in dilute sulfuric acid 5 minutes, remove the Nano silver grain mask, obtain the ring-type assembly of golden nanometer particle in polyelectrolyte edge.
Claims (10)
1. realize that in the edge of mask nanoparticle surface induces the method for self assembly for one kind, its step is as follows:
(a) on substrate, be fixed for the template of constructing micrometre or nanostructured;
(b) carry out the deposition of polyelectrolyte layer on template, polyelectrolyte is a polydiene propyl-dimethyl ammonium chlorine;
(c) the fixing mask on the surface of polyelectrolyte layer, the particle diameter of mask nano particle is 10～100 nanometers, mask thicknesses is suitable with the mask nano particle diameter;
(d) remove the template of introducing by in the step (a), at substrate surface, originally there was the zone of template to expose out, originally there was not the zone of template then to keep the double-decker of polyelectrolyte and mask nano particle, simultaneously expose polyelectrolyte layer, thereby obtain the alternately periodic structure of arrangement of double-decker and exposed substrate surface in mask edge;
(e) on the polyelectrolyte layer that mask edge exposes, assemble and the different types of nano particle of mask nano particle by electrostatic interaction, thereby induce self assembly in edge's realization nanoparticle surface of mask.
2. a kind of edge at mask as claimed in claim 1 realizes that nanoparticle surface induces the method for self assembly, and it is characterized in that: the substrate in the step (a) is quartz plate, silicon chip, sheet glass or macromolecule substrate, uses after the substrate surface cleaning.
3. a kind of edge at mask as claimed in claim 1 realizes that nanoparticle surface induces the method for self assembly, it is characterized in that: the template that is used in constructing micrometre or nanostructured with physics spin coating method or Chemical Crosslinking Methods that fixedly is meant in the step (a) is fixed on the substrate.
4. a kind of method of inducing self assembly in edge's realization nanoparticle surface of mask as claimed in claim 1, it is characterized in that: the mould material in the step (a) is polystyrene colloid microballoon, silicon dioxide colloid microballoon or dimethyl silicone polymer, and the cycle of template is 100 nanometers～100 micron; Template is micro-sphere structure or list structure, and it is 50 nanometers～1 millimeter that template is fixed on behind the substrate surface thickness.
5. a kind of method of inducing self assembly in edge's realization nanoparticle surface of mask as claimed in claim 1, it is characterized in that: the polyelectrolyte layer deposition in the step (b) is meant by chemical action power or physical force and makes the polyelectrolyte compound be adsorbed onto substrate and template surface, thickness 0.5～1.5 nanometer.
6. a kind of method of inducing self assembly in edge's realization nanoparticle surface of mask as claimed in claim 1, it is characterized in that: the mask in the step (c) is meant one deck organic material nano particle or inorganic material nano particle is covered substrate surface and template surface by physics or chemisorption, the organic material nano particle is a polymethylacrylic acid or poly-to vinylbenzenesulfonic acid, and the inorganic material nano particle is gold, silver, copper, CdTe, CdS, ZnO, Fe
2O
3Or Fe
3O
4
7. a kind of edge at mask as claimed in claim 1 realizes that nanoparticle surface induces the method for self assembly, it is characterized in that: said in the step (d) removed template and is meant with chemical attack or physical etchings method and removes the template that is used for constructing micrometre or nanostructured.
8. a kind of edge at mask as claimed in claim 1 realizes that nanoparticle surface induces the method for self assembly, it is characterized in that: the said static self assembly of step (e) is meant based on the electrostatic attraction of the polyelectrolyte of oppositely charged and nano particle with as the assemble method of driving force.
9. a kind of method of inducing self assembly in edge's realization nanoparticle surface of mask as claimed in claim 1, it is characterized in that: step (e) said on the polyelectrolyte layer that mask edge exposes the assembling with the different types of nano particle of mask nano particle be organic material nano particle or inorganic material nano particle, the organic material nano particle is a polymethylacrylic acid or poly-to vinylbenzenesulfonic acid, and the inorganic material nano particle is gold, silver, copper, CdTe, CdS, ZnO, Fe
2O
3Or Fe
3O
4
10. a kind of method of inducing self assembly in edge's realization nanoparticle surface of mask as claimed in claim 1, it is characterized in that: further utilize the method for chemical attack or physical etchings to remove mask, only stay the assembly of nano particle, thereby induce self assembly in edge's realization nanoparticle surface of mask along mask edge.
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Cited By (7)
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| CN102294213A (en) * | 2011-07-06 | 2011-12-28 | 吉林大学 | Preparation method of polymer-coated binary double-functional nano-cluster core-shell microspheres |
| WO2013164741A1 (en) * | 2012-04-30 | 2013-11-07 | International Business Machines Corporation | Methods and apparatuses for positioning nano-objects with aspect ratios |
| CN104517616A (en) * | 2013-10-07 | 2015-04-15 | 株式会社东芝 | Pattern formation method and magnetic recording medium manufacturing method |
| CN106033719A (en) * | 2015-03-18 | 2016-10-19 | 中芯国际集成电路制造(上海)有限公司 | Formation method of semiconductor structure |
| CN109963409A (en) * | 2019-04-10 | 2019-07-02 | 京东方科技集团股份有限公司 | The manufacturing method and board structure of substrate side surfaces conducting wire |
| CN111326951A (en) * | 2020-03-11 | 2020-06-23 | 吉林大学 | Perovskite micro-ring resonator array, preparation method and application thereof |
| CN111704894A (en) * | 2020-06-04 | 2020-09-25 | 东华大学 | Assembling preparation method of efficient solar heating surface |
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2010
- 2010-11-11 CN CN2010105392896A patent/CN102020241A/en active Pending
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| CN102294213A (en) * | 2011-07-06 | 2011-12-28 | 吉林大学 | Preparation method of polymer-coated binary double-functional nano-cluster core-shell microspheres |
| CN104272451B (en) * | 2012-04-30 | 2017-03-29 | 国际商业机器公司 | For the method and apparatus of nanometer object of the positioning with aspect ratio |
| WO2013164741A1 (en) * | 2012-04-30 | 2013-11-07 | International Business Machines Corporation | Methods and apparatuses for positioning nano-objects with aspect ratios |
| GB2515217A (en) * | 2012-04-30 | 2014-12-17 | Ibm | Methods and apparatuses for positioning nano-objects with aspect ratios |
| US9121108B2 (en) | 2012-04-30 | 2015-09-01 | International Business Machines Corporation | Methods and apparatuses for positioning nano-objects with aspect ratios |
| GB2515217B (en) * | 2012-04-30 | 2016-09-07 | Ibm | Methods and apparatuses for positioning nano-objects with aspect ratios |
| CN104517616A (en) * | 2013-10-07 | 2015-04-15 | 株式会社东芝 | Pattern formation method and magnetic recording medium manufacturing method |
| CN106033719A (en) * | 2015-03-18 | 2016-10-19 | 中芯国际集成电路制造(上海)有限公司 | Formation method of semiconductor structure |
| CN109963409A (en) * | 2019-04-10 | 2019-07-02 | 京东方科技集团股份有限公司 | The manufacturing method and board structure of substrate side surfaces conducting wire |
| WO2020207465A1 (en) * | 2019-04-10 | 2020-10-15 | 京东方科技集团股份有限公司 | Method for manufacturing wire on side surface of substrate and substrate structure |
| CN109963409B (en) * | 2019-04-10 | 2021-02-23 | 京东方科技集团股份有限公司 | Manufacturing method of substrate side surface wire and substrate structure |
| US11984546B2 (en) | 2019-04-10 | 2024-05-14 | Beijing Boe Display Technology Co., Ltd. | Method for manufacturing side wire for substrate and substrate structure |
| CN111326951A (en) * | 2020-03-11 | 2020-06-23 | 吉林大学 | Perovskite micro-ring resonator array, preparation method and application thereof |
| CN111704894A (en) * | 2020-06-04 | 2020-09-25 | 东华大学 | Assembling preparation method of efficient solar heating surface |
| CN111704894B (en) * | 2020-06-04 | 2021-07-20 | 东华大学 | Assembling preparation method of efficient solar heating surface |
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Application publication date: 20110420 |