CN103227102B - A kind of graphical nano-particles self assemble manufacture method - Google Patents
A kind of graphical nano-particles self assemble manufacture method Download PDFInfo
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- CN103227102B CN103227102B CN201310133783.6A CN201310133783A CN103227102B CN 103227102 B CN103227102 B CN 103227102B CN 201310133783 A CN201310133783 A CN 201310133783A CN 103227102 B CN103227102 B CN 103227102B
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Abstract
The present invention relates to a kind of graphical nano-particles self assemble manufacture method, its step includes: adopts single-sided polishing monocrystalline substrate, deposits out one layer of parylene film by chemical gas-phase deposition method in surface of silicon; By conventional photolithographic method, make required photoresist mask graph in surface of silicon; Adopt oxygen plasma etch method, etch exposed parylene film; Adopt diamond dicing saw that silicon substrate is carried out scribing; Acetone is adopted to remove the photoresist in surface of silicon; Silicon substrate after removing photoresist is immersed in the mixed liquor of concentrated sulphuric acid, hydrogen peroxide, cleans with deionized water after taking-up; Take a certain amount of nano-particle suspension prepared, be added dropwise to equipped with, in the container of ethanol, two kinds of liquid mixing uniformly and being poured slowly in the culture dish having been loaded with deionized water; After the silicon substrate obtained is fully immersed in the liquid in culture dish, takes out and be placed in another culture dish, and level puts into a drying baker, obtains the silicon substrate with graphical nano-particles self assemble at ambient temperature after natural evaporation.
Description
Technical field
The present invention relates to a kind of graphical nano-particles self assemble manufacture method, utilize nano-particle evaporation-induced self-assembly phenomenon especially with regard to one, prepare the manufacture method of hydrophilic and hydrophobic silicon substrate aided nano particles self assemble.
Background technology
Self assembly (self-assembly) refers to the construction unit such as molecule and nano-particle in equilibrium conditions, is spontaneously concluded into the process of that determine in thermodynamically stable, structure, special in performance aggregation by non-covalent bond effect. The maximum process that feature is self assembly of self assembly once, will automatically proceed to certain intended terminal, auto arrangement is become orderly figure by the construction unit such as molecule, even forming the effect also without external force of the complicated ergasia. Self assembly can form monolayer, film, vesicle, micelle, micro-pipe, spillikin and more complicated organic-metallic, organic and inorganic, biology-abiotic complex etc., and its multiformity exceedes the material prepared by other method. The self assembly arrangement method of nano-particle has a variety of, and dividing by realization means mainly has: dip coated, rotary coating, electrophoretic deposition and evaporation self assembly etc.
During evaporation self assembly, the substrate through suitably processing is immersed in nano-particle suspension (or being dripped over the substrate surface by suspension), controls the temperature of surrounding, humidity, gas flow rate etc., make suspension evaporate at a constant speed. When liquid level thickness is close or less than nano-particle diameter, nano-particle will precipitate out gradually, the factor such as surface tension and Van der Waals force forces them to be fixed on substrate surface close-packed arrays, thus obtaining the regular nano-grain array with special construction on substrate. Compared with other self assembly arrangement method, evaporation self-assembling method has significant advantage in the systematicness of operability and rank results. But the substrate owing to adopting be single-sided polishing, surface without the monocrystalline silicon piece of other structure, prepared nano-particle close-packed configuration is distributed on whole substrate surface, and without specific figure. Therefore, this self-assembling method controllability is poor, it is difficult to graphical, restricted application.
Summary of the invention
For the problems referred to above, the invention aims to improve the controllability of nano-particles self assemble process, realize graphical arrangement, it is proposed that hydrophilic and hydrophobic silicon substrate aided nano particles self assemble manufacture method.
For achieving the above object, the present invention takes techniques below scheme: a kind of graphical nano-particles self assemble manufacture method, it comprises the following steps: 1) adopts 4 inches of single-sided polishing monocrystalline substrate, deposits out one layer of parylene film by chemical gas-phase deposition method in surface of silicon; 2) by conventional photolithographic method, required photoresist mask graph is made in surface of silicon; 3) adopt oxygen plasma etch method, etch exposed parylene film; 4) adopt diamond dicing saw that silicon substrate is carried out scribing; 5) acetone is adopted to remove the photoresist in surface of silicon; 6) by silicon substrate the concentrated sulphuric acid that temperature is 120 DEG C, hydrogen peroxide mixed liquor in soak 10 minutes, after taking-up with deionized water clean 5～10 times; 7) take the nano-particle suspension prepared of 10～15uL, be added dropwise in the container equipped with 1mL ethanol, two kinds of liquid mixing uniformly and are poured slowly in the culture dish having been loaded with deionized water; 8), after the silicon substrate that step 6) obtains is fully immersed in the liquid in culture dish, takes out and be placed in another culture dish, and level puts into a drying baker, at ambient temperature after natural evaporation, namely obtains the silicon substrate with graphical nano-particle.
Described step 2) in, photoresist mask thickness is 1.0 μm～2.0 μm.
In described step 3), parylene film thickness is 50nm～150nm.
In described step 6), the mass fraction of hydrogen peroxide is 40%, and the volume ratio of concentrated sulphuric acid and hydrogen peroxide is 4:1.
Nano-particle suspension in described step 7) is polystyrene nanoparticles suspension.
Nano-particle suspension in described step 7) is nano SiO 2 particle suspension.
In described step 8), in drying baker, pass into nitrogen accelerate evaporation.
Due to the fact that and take above technical scheme, it has the advantage that 1, the present invention utilizes the hydrophilic and hydrophobic difference of surface of silicon to make nano-particles self assemble be positioned at restriction region, solve nano-particles self assemble controllability poor and be difficult to patterned problem, improve the range of application of self-assembling technique, making the operability of the present invention, controllability have clear superiority with the systematicness of rank results compared with other self-assembling method, particularly in preparing patterned rule solid matter nano-grain array, its effect is difficult to substitute. 2, the oxygen plasma dry method used in the present invention removes photoresist technology and conventional lithographic techniques will originate from microelectronic manufacturing technology, therefore can conveniently realize batch and parallel fabrication. 3, the present invention adopts evaporation self-assembling method, simple to operate, present invention can be widely used in fields such as photoelectron, bio-pharmaceuticals, chemical industry, and some field is produced not predictable facilitation.
Accompanying drawing explanation
Fig. 1 is Grown parylene film schematic diagram of the present invention
Fig. 2 is that the present invention defines photoresist mask graph by conventional photolithography; Fig. 2 a is that the present invention scribbles photoresist mask schematic diagram; Fig. 2 b is by schematic diagram after conventional photolithography photoetching photoresist mask
Fig. 3 is the schematic diagram after present invention oxygen plasma etch parylene film
Fig. 4 is the patterned substrate schematic diagram obtaining after acetone of the present invention removes photoresist having hydrophilic difference
Fig. 5 is that the present invention is evaporated self assembly schematic diagram on patterned substrate basis
Fig. 6 is the graphical nano-particles self assemble schematic diagram that the present invention finally realizes
Fig. 7 is the schematic top plan view of Fig. 6
Fig. 8 is the ultramicroscope design sketch of the graphical nano-particles self assemble arrangement result obtained by the inventive method;Fig. 8 a is the ultramicroscope design sketch of nano-particles self assemble of the present invention arrangement result; Fig. 8 b is the partial enlarged drawing of Fig. 8 a
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in detail.
1) as it is shown in figure 1, prepare 4 inches of single-sided polishing monocrystalline substrate 1, strata xylol (Parylene) thin film 2 is gone out by chemical vapor deposition (ChemicalVaporDeposition-CVD) method at silicon substrate 1 surface deposition.
2) as shown in Figure 2, pass through conventional photolithographic method, spin coating photoresist 3 mask (as shown in Figure 2 a) on silicon substrate 1 surface, according still further to the production order of whirl coating, front baking, exposure, after bake and development, makes required photoresist 3 mask graph (as shown in Figure 2 b) on silicon substrate 1 surface;
Wherein, photoresist 3 mask thickness is 1.0 μm～2.0 μm.
3) as it is shown on figure 3, adopt oxygen plasma etch method, exposed parylene film 2 is etched.
Wherein, the oxygen gas plasma stripping machine that the present invention adopts is when etching photoresist 3 mask and parylene film 2, and etching speed is of substantially equal, is about 3nm/s; And photoresist 3 mask thickness is much larger than parylene film 2, therefore when exposed parylene film 2 is completely removed, photoresist 3 mask still exists on silicon substrate 1 surface with parylene film 2.
Wherein, parylene film 2 thickness is 50nm～150nm.
4) adopt diamond dicing saw, by step pitch 1cm × 1cm, silicon substrate 1 is carried out scribing;
5) as shown in Figure 4, step 3) the silicon substrate 1 with photoresist 3 mask and parylene film 2 obtained adopts acetone remove photoresist 3 mask on this silicon substrate 1 surface, obtains the silicon substrate 1 with the patterned surface of hydrophilic and hydrophobic difference.
Wherein, silicon substrate 1 surface exposed is activated and very hydrophilic by oxygen plasma, and is photo-etched the parylene film 2 surface relative hydrophobic of glue 3 protection.
6) conventional cleaning, soaks silicon substrate 1 10 minutes in the concentrated sulphuric acid of 120 DEG C, the mixed liquor of hydrogen peroxide, cleans 5～10 times with deionized water after taking-up;
Wherein, mixed liquor hydrogen peroxide mass fraction is 40%, and the volume ratio of concentrated sulphuric acid and hydrogen peroxide is 4:1.
7) configuration nano-particle suspension 4, with the shifting liquid meter that range is 20uL～200uL, take 10～15uL nano-particle suspension 4 configured, be added dropwise in the container equipped with 1mL ethanol, two kinds of liquid mixing uniformly and are poured slowly in the culture dish having been loaded with deionized water.
Wherein, owing to there being the existence of ethanol in culture dish, nano-particle suspension 4 will disperse rapidly in deionized water, make nano-particle 5 can be arranged in equably after evaporation on silicon substrate 1 surface;
Wherein, nano-particle suspension 4 carries out deionized water dilution by nano-particle original solution and obtains, and nano-particle original solution is commercially available prod; In nano-particle suspension 4, the amount of deionized water is that the concentration according to nano-particle original solution and the suspension needing configuration is calculated, in order to realize the packed mono-layer of nano-particle, the concentration of the nano-particle suspension configured is typically about in every milliliter of suspension containing 1 × 1012～8 × 1012Individual nano-particle; Concentration is for reference only herein, needs repetition test in practical operation, to seek optimum concentration range. Nano-particle suspension 4 is applicable to nano SiO 2 particle suspension, is also applied for polystyrene nanoparticles suspension;Nano-particle suspension contains multiple nano-particle diameter, from 250nm～940nm not etc.
8) silicon substrate 1 after step 6) being cleaned is soaked in the nano-particle suspension 4 configured by step 7) at ambient temperature, is fully immersed in after nano-particle suspension 4 until silicon substrate 1 and just can take out. As it is shown in figure 5, due to the difference of hydrophilic and hydrophobic, nano-particle suspension 4 is by the hydrophilic region being limited at silicon substrate 1 surface, and parylene film 2 surface of relative hydrophobic is then adhered to without nano-particle suspension 4; The silicon substrate 1 processed is lain in a horizontal plane in another culture dish, this culture dish level is put into a drying baker, natural evaporation at ambient temperature, just can evaporate in general 24 hours.
Wherein, drying baker is possible to prevent this culture dish of the contaminants in air; Additionally, nano-particle suspension 4 can also pass through nitrogen accelerates evaporation.
As shown in Figure 6, Figure 7, after nano-particle suspension 4 evaporates completely, take out silicon substrate 1; Under the effect of the factor such as surface tension and Van der Waals force, nano-particle 5 is fixed in an orderly manner to be had on hydrophilic silicon substrate 1 surface (as shown in Figure 8).
The invention solves the location arrangement problem of nano-particle 5 self assembly in restriction region, namely a fixed structure is obtained in specific position, propose and achieve hydrophilic and hydrophobic silicon substrate 1 aided nano granule 5 self assembly manufacture method, solve nano-particles self assemble controllability well poor and be difficult to patterned problem, improve the scope of application of self assembly.
The various embodiments described above are merely to illustrate the present invention, and wherein the structure of each parts, connected mode etc. all can be varied from, every equivalents carried out on the basis of technical solution of the present invention and improvement, all should not get rid of outside protection scope of the present invention.
Claims (8)
1. a graphical nano-particles self assemble manufacture method, it comprises the following steps:
1) adopt 4 inches of single-sided polishing monocrystalline substrate, deposit out one layer of parylene film by chemical gas-phase deposition method in surface of silicon;
2) by conventional photolithographic method, required photoresist mask graph is made in surface of silicon;
3) adopt oxygen plasma etch method, etch exposed parylene film;
4) adopt diamond dicing saw that silicon substrate is carried out scribing;
5) acetone is adopted to remove the photoresist in surface of silicon;
6) by silicon substrate the concentrated sulphuric acid that temperature is 120 DEG C, hydrogen peroxide mixed liquor in soak 10 minutes, after taking-up with deionized water clean 5～10 times;
7) the nano-particle suspension prepared of 10～15uL is taken, it is added dropwise in the container equipped with 1mL ethanol, uniformly and being poured slowly in the culture dish having been loaded with deionized water by two kinds of liquid mixing, the concentration of nano-particle suspension is containing 1 × 10 in every milliliter of suspension12～8 × 1012Individual nano-particle;
8) by step 6) silicon substrate that obtains be fully immersed in culture dish liquid after, take out and be placed in another culture dish, and level puts into a drying baker, at ambient temperature after natural evaporation, namely obtains the silicon substrate with graphical nano-particle.
2. a kind of graphical nano-particles self assemble manufacture method as claimed in claim 1, it is characterised in that: described step 2) in, photoresist mask thickness is 1.0 μm～2.0 μm.
3. a kind of graphical nano-particles self assemble manufacture method as claimed in claim 1, it is characterised in that: described step 3) in, parylene film thickness is 50nm～150nm.
4. a kind of graphical nano-particles self assemble manufacture method as claimed in claim 2, it is characterised in that: described step 3) in, parylene film thickness is 50nm～150nm.
5. a kind of graphical nano-particles self assemble manufacture method as claimed in claim 1 or 2 or 3 or 4, it is characterised in that: described step 6) in, the mass fraction of hydrogen peroxide is 40%, and the volume ratio of concentrated sulphuric acid and hydrogen peroxide is 4:1.
6. a kind of graphical nano-particles self assemble manufacture method as claimed in claim 1 or 2 or 3 or 4, it is characterised in that: described step 7) in nano-particle suspension be polystyrene nanoparticles suspension.
7. a kind of graphical nano-particles self assemble manufacture method as claimed in claim 1 or 2 or 3 or 4, it is characterised in that: described step 7) in nano-particle suspension be nano SiO 2 particle suspension.
8. a kind of graphical nano-particles self assemble manufacture method as claimed in claim 1 or 2 or 3 or 4, it is characterised in that: described step 8) in, in drying baker, pass into nitrogen accelerate evaporation.
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| CN110203878A (en) * | 2019-05-27 | 2019-09-06 | 东南大学 | Single layer nano particle dimer and poly preparation based on hydrophobe array |
| CN113184803B (en) * | 2021-04-22 | 2022-07-12 | 西安交通大学 | Magnetic nanoparticle self-assembly system based on magnetic field driving and processing method |
| CN113336185A (en) * | 2021-05-21 | 2021-09-03 | 大连理工大学 | Method for processing trans-scale micro-nano structure integrated with nano raised array |
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| CN1656264A (en) * | 2002-03-25 | 2005-08-17 | 北卡罗来纳-查佩尔山大学 | Method for assembling nano objects |
| CN1802727A (en) * | 2003-03-21 | 2006-07-12 | 北卡罗来纳-查佩尔山大学 | Methods and apparatus for patterned deposition of nanostructure-containing materials by self-assembly and related articles |
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| CN1656264A (en) * | 2002-03-25 | 2005-08-17 | 北卡罗来纳-查佩尔山大学 | Method for assembling nano objects |
| CN1802727A (en) * | 2003-03-21 | 2006-07-12 | 北卡罗来纳-查佩尔山大学 | Methods and apparatus for patterned deposition of nanostructure-containing materials by self-assembly and related articles |
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