CN108483390B - A kind of printing process of functionality micro-nano heterojunction structure - Google Patents
A kind of printing process of functionality micro-nano heterojunction structure Download PDFInfo
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- CN108483390B CN108483390B CN201810187798.3A CN201810187798A CN108483390B CN 108483390 B CN108483390 B CN 108483390B CN 201810187798 A CN201810187798 A CN 201810187798A CN 108483390 B CN108483390 B CN 108483390B
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- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
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Abstract
The invention discloses a kind of printing processes of micro-nano heterojunction structure.This method includes the following steps: that organic phase nanomaterial assembly liquid uniformly 1) is spread over silicon column template surface, then substrate is covered in the silicon column template, so that the solvent in the organic phase nanomaterial assembly liquid is volatilized, just forms the dot matrix array structure of regularly arranged depositing nano-materials on the substrate；2) water phase nanomaterial assembly liquid is injected into the silicon column template, the water in the water phase nanomaterial assembly liquid is set to volatilize, nano material is just deposited in the substrate with regular linear array structure, finally forms the micro-nano heterojunction structure of dotted line connection on the substrate.This printing process can be realized heterojunction structure in substrate large area printing, make its micro-nano electronic circuit, optical element, in terms of all have potential application.
Description
Technical field
The present invention relates to a kind of printing processes of functional micro-nano heterojunction structure.
Background technique
Functional dotted line micro-nano structure is the basic function for constituting many optical elements, microelectronic circuit and sensor
Unit has potential huge applications value in terms of industrial application.Particularly, dotted line micro-nano structure is connected in a manner of lateral,
It is capable of the property of reasonable binding function dotted line micro-nano structure, provides what single functional dotted line micro-nano structure did not had
Physical characteristic.In the connection of dotted line micro-nano structure, the connection type of dotted line micro-nano unit is particularly important.Dotted line micro-nano knot
The novel interface that structure junction occurs is concerned in the research of heterojunction structure in recent years, provides many wounds for heterojunction structure
The function of new property.For the dotted line micro-nano structure connection type prepared a little around line, it is embedding that point is distributed online surface or point
Enter the connection types such as online both ends.
Traditional photolithography method, which prepares micro-nano structure and needs a person with the qualifications of a general, to be expected inevitably to be exposed under light or energy source, because
This photoetching process prepares micro-nano structure and is limited by very large.For comparing, solwution method (carve by printing, solution assembling, wet process
Erosion) it is one kind selection very well for substituting conventional photolithography and preparing micro-nano structure.The applicable material ranges of solwution method are wide, enumerate
From inorganic nanoparticles to organic biomolecules etc..And the heterogeneous micro-nano structure of more materials composition can be by the solution of iteration at
The preparation of reason method, such as combine the inkjet printing methods of repeatability that can prepare optical detector by more material inks, two steps
Solution capillary flow assemble method prepares double-colored grid.However, solwution method prepares a greatest difficulty present in micro-nano structure is
It is difficult to manipulate in solution flow process, especially solution is when micro-nano structure surface flows, it is easy to cause heterojunction structure even
It meets place and forms chaotic connection type.In general, the interaction of functional material and solution properties is common in micro- liquid environment
Determine prepared micro-nano structure.It is accurate to manipulate solution flowing with important during solwution method prepares heterojunction structure
Meaning.On the one hand studying fine solution flowing is to explore the method for preparing heterogeneous micro-nano structure, also to the spy of this class formation
Different physicochemical properties are studied, and are ready work for the potential application of these new properties；On the other hand can also add
Deep people combine the research of this respect to carry out the exploration more deep to this system the understanding of heterogeneous micro-nano structure.This is not
But there is scientific meaning, and there is important application value.
Summary of the invention
An object of the present invention is to provide a kind of printing process of micro-nano heterojunction structure.
The printing process of micro-nano heterojunction structure provided by the present invention is by two different kinds of nanomaterial assembly liquid
As ink, assembles concentration is successively printed onto base in the form of micro-nano point cable architecture according to the pattern and arrangement of design by Lithographic template
On bottom.
Specifically include the following steps:
1) organic phase nanomaterial assembly liquid is uniformly spread over into silicon column template surface, substrate is then covered into the silicon
On column template, so that the solvent in the organic phase nanomaterial assembly liquid is volatilized, just form on the substrate regularly arranged
Depositing nano-materials dot matrix array structure；
2) water phase nanomaterial assembly liquid is injected into the silicon column template, is made in the water phase nanomaterial assembly liquid
Water volatilization, nano material just deposits in the substrate with regular linear array structure, finally shape on the substrate
The micro-nano heterojunction structure connected at the dotted line of large area.
In above-mentioned steps 1) in, after the liquid film and template contacts of the organic phase nanomaterial assembly liquid, liquid film is in silicon column
Volatilize under template-mediated, be initially formed continuous liquid bridge, due to Rayleigh, Taylor is unstable, liquid bridge therefrom between be broken, in substrate.Institute
The liquid bridge stated is with the evaporation of solvent in organic phase nanomaterial assembly liquid, and liquid film is retracted into along the silicon column on Lithographic template
The fluid passage of regular array.The liquid bridge fracture is with the evaporation of solvent in organic phase nanomaterial assembly liquid, liquid
Under the induction of photoetching silicon column template, Rayleigh Taylor unstability occurs bridge for centre, is shrunk to dot matrix liquid film along silicon column.
In above method step 2), the suitable viscosity of water phase nanomaterial assembly liquid and surface tension make liquid bridge stablize receipts
Contracting, nano material are just assembled into substrate with accurate orderly linear array again.The dotted line of large area is finally formed on the substrate
The micro-nano heterojunction structure of connection, and the connection type controllable precise between dotted line.
In above method step 1), the template is that a kind of reusable photoetching silicon column template is replaced printing machine
In pattern reel or galley, play the role of induce nanomaterial assembly.
It is thin that the substrate can be but be not limited to silicon wafer, sheet glass, quartz plate, iron plate, copper sheet, PDMS film, PET
One of film, PS film, PU film, PI film, aluminium flake, alumina wafer.
The nanomaterial assembly liquid is uniformly to be layered on silicon by the liquid-transfering gun apart from photoetching silicon column template surface certain distance
Column template surface.
The dot matrix array structure is to form the similar silicon column pattern with certain altitude according to the design of silicon column template
Depositing array.
The linear array structure is to form the depositing array with certain length according to the design of silicon column template.
The assembles concentration of the organic phase nano material is made of nano material and organic solvent, wherein the nano material
Mass content be 0.01%~10% (preferably 0.1%~1%), surplus is solvent.
The assembles concentration of the water phase nano material is made of nano material, surfactant and aqueous solvent, wherein described
The mass content of nano material is 0.01%~10% (preferably 0.1%~1%), and the mass content of surfactant is
0.005%~1% (preferably 0.1%~0.5%), surplus is water.
The particle size range of the nano material is 2nm~900nm.
Nano material in the organic phase can be but be not limited only to polymer (such as PS, polyaniline), quantum dot
(CdS), one or more of organic fluorescence molecule, function small molecule.
Nano material in the water phase can be but be not limited to colloid micro ball (polystyrene microsphere), nano particle
(platinum, gold, silver, copper, zinc oxide, iron oxide, ferroso-ferric oxide, titanium dioxide, silica, CdTe quantum, CdS), carbon are received
One or more of mitron, graphene, polymer (such as polyvinyl alcohol).
The micro-nano heterojunction structure of the dotted line connection is the array structure of the array structure of line crossing point, line cladding point respectively
Or line is by an array structure for partition.
When the concentration of nano material in organic phase nanomaterial assembly liquid is 0.01%-0.1%, usually it is prepared
It is the array structure of line crossing point；The concentration for improving nano material in organic phase nanomaterial assembly liquid, when its concentration is
When 0.2%-0.5%, what is be usually prepared is the array structure of line cladding point；Further increase organic phase nanomaterial assembly
The concentration of nano material in liquid, when its concentration is 0.6%-1%, what is be usually prepared is line by an array junctions for partition
Structure.
The surfactant can be but be not limited to anionic surfactant such as sodium dodecyl benzenylsulfonate, ten
Sodium dialkyl sulfate, stearic acid, cationic surfactant such as quaternary ammonium compound, zwitterionic surfactant such as amino acid
Type, betaine type, polyacrylamide, lecithin and nonionic surfactant for example fatty acid sorbitan, fatty glyceride,
At least one of polysorbate, tween.
The organic solvent can be but not limited to toluene, o-dichlorohenzene, chlorobenzene, dimethylbenzene, dimethylformamide, and four
Chlorination carbon, octane, heptane, n-hexane, one or more of petroleum ether, methyl pyrrolidone.
Specifically, the assembles concentration of the organic phase nano material can are as follows: 1) by the CdS quantum dot of partial size 5nm, polystyrene
The CdS mass content prepared with o-dichlorohenzene is 0.2%, and the mass content of polystyrene is 0.1%-1%, surplus is adjacent
The assembles concentration of dichloro-benzenes；Or 2) the saturation polyaniline assembles concentration prepared by polyaniline, methyl pyrrolidone.
Specifically, the assembles concentration of the water phase nano material can are as follows: 1) by the CdS quantum dot of partial size 5nm, polyvinyl alcohol,
The assembles concentration of lauryl sodium sulfate and water preparation, wherein CdS mass content is 0.2%, and the mass content of polyvinyl alcohol is
0.5%, the mass content of lauryl sodium sulfate is 0.2%, and surplus is water；2) by the Nano silver grain of partial size 30nm, 12
The mass content for the silver nano-grain that sodium alkyl sulfate is prepared with water is 10%, the mass content of lauryl sodium sulfate is
0.2%, surplus is the assembles concentration containing Nano silver grain of water；3) by partial size be about 180nm polystyrene sphere, dodecane
The polystyrene sphere mass content that base sodium sulphate is prepared with water is 1%, the mass content of lauryl sodium sulfate is
0.2%, surplus is the assembles concentration of water.
The micro-nano heterojunction structure that the above method is prepared also belongs to protection scope of the present invention.
The present invention utilizes nanomaterial assembly by the way that different nanomaterial assembly liquid to be introduced into photoetching silicon column template
The different designs of pattern and spread pattern of the heterogeneity and silicon column of liquid in template, can scale preparation large area it is micro-
The heterojunction structure of dotted line of receiving connection.
The present invention using photoetching silicon column template by different types of nanomaterial assembly liquid be successively printed on plane or
On curved surface, the heterogeneous micro-nano structure of dotted line connection is prepared.Such dotted line junction interface pattern controllable precise, is avoided that solution
It is disorderly and unsystematic to prepare interface pattern in more material micro-nano structures.Conventional photolithography is replaced to prepare micro-nano heterojunction structure letter with the method
It is single quick, it is flexibly easy-to-use, convenient for the large-scale production of micro-structure demand.The micro-nano structure array of dotted line connection prepared by the present invention
The controllable precise that can be realized dotted line interface has potential application in terms of microelectronic circuit, optical element, senser element
Value.
Detailed description of the invention
Fig. 1 is that photoetching silicon column template of the present invention successively induces two kinds of nanomaterial assembly liquid to form showing for point wire connection structure
It is intended to.
Fig. 2 is in 1-3 of the embodiment of the present invention, and photoetching circle silicon column template successively induces two kinds of nanomaterial assembly liquid in silicon
The scanning electron microscope diagram piece and laser co-focusing picture of the three kinds of point wire connection structures formed in substrate.
Fig. 3 is in the embodiment of the present invention 4, and photoetching diamond shape silicon column template successively induces two kinds of nanomaterial assembly liquid in silicon substrate
The laser co-focusing picture of the point wire connection structure formed on bottom and the scanning electron microscope diagram of photoetching diamond shape silicon column template
Piece.
Fig. 4 is in 1-5 of the embodiment of the present invention, and the circle of photoetching, diamond shape and star silicon column template successively induce two kinds to receive
The laser co-focusing picture for the point wire connection structure that rice material assembles concentration is formed on a silicon substrate.
Fig. 5 is in the embodiment of the present invention 3,6, and the round silicon column template of photoetching successively induces two kinds of nanomaterial assembly liquid to exist
The point wire connection structure formed in silicon base, the corresponding diagram that wire connection structure detects the propagation of light and ammonia.
Specific embodiment
Method of the invention is illustrated below by specific embodiment, but the present invention is not limited thereto, it is all at this
Any modifications, equivalent replacements, and improvements etc. done within the spirit and principle of invention, should be included in protection model of the invention
Within enclosing.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1
It is by the CdS mass content prepared by the CdS quantum dot of partial size 5nm, polystyrene and o-dichlorohenzene
0.2%, the assembles concentration that the mass content of polystyrene is 0.1%, surplus is o-dichlorohenzene takes 10 microlitres of uniformly pavings by liquid-transfering gun
Exhibition is in the round silicon column template of photoetching；Silicon base is covered and is covered in the silicon column template of assembles concentration, makes solvent at 80 DEG C
Uniformly volatilization；It is cooling that withdrawing device places room temperature, re-injects 10 microlitres of CdS quantum dots by partial size 5nm, polyvinyl alcohol, and ten
The assembles concentration of sodium dialkyl sulfate and water preparation, wherein CdS mass content is 0.2%, and the mass content of polyvinyl alcohol is
0.5%, the mass content of lauryl sodium sulfate is 0.2%, and surplus is water, and solvent is made uniformly to volatilize at 50 DEG C, to be assembled
After water volatilization in liquid, the micro-nano connection structure that line passes through circular dot is obtained in the silicon wafer with flat surface.
Embodiment 2
By by the CdS quantum dot of partial size 5nm, the CdS mass content that polystyrene is prepared with o-dichlorohenzene is
0.2%, the assembles concentration that the mass content of polystyrene is 0.5%, surplus is o-dichlorohenzene takes 10 microlitres of uniformly pavings by liquid-transfering gun
Exhibition is in the round silicon column template of photoetching；Silicon base is covered and is covered in the silicon column template of assembles concentration, makes solvent at 80 DEG C
Uniformly volatilization；It is cooling that withdrawing device places room temperature, re-injects 10 microlitres of CdS quantum dots by partial size 5nm, polyvinyl alcohol, and ten
The assembles concentration of sodium dialkyl sulfate and water preparation, wherein CdS mass content is 0.2%, and the mass content of polyvinyl alcohol is
0.5%, the mass content of lauryl sodium sulfate is 0.2%, and surplus is water, and solvent is made uniformly to volatilize at 50 DEG C, to be assembled
After water volatilization in liquid, the micro-nano connection structure of line cladding circular dot is obtained in the silicon wafer with flat surface.
Embodiment 3
By by the CdS quantum dot of partial size 5nm, the CdS mass content that polystyrene is prepared with o-dichlorohenzene is
0.2%, the assembles concentration that the mass content of polystyrene is 1%, surplus is o-dichlorohenzene takes 10 microlitres uniformly to sprawl by liquid-transfering gun
In the round silicon column template of photoetching；Silicon base is covered and is covered in the silicon column template of assembles concentration, keeps solvent equal at 80 DEG C
Even volatilization；It is cooling that withdrawing device places room temperature, re-injects 10 microlitres of CdS quantum dots by partial size 5nm, polyvinyl alcohol, and 12
The assembles concentration of sodium alkyl sulfate and water preparation, wherein CdS mass content is 0.2%, and the mass content of polyvinyl alcohol is 0.5%,
The mass content of lauryl sodium sulfate is 0.2%, and surplus is water, so that solvent is uniformly volatilized at 50 DEG C, in liquid to be assembled
After water volatilization, the micro-nano connection structure of line connection circular dot is obtained in the silicon wafer with flat surface.
Embodiment 4
By by the CdS quantum dot of partial size 5nm, the CdS mass content that polystyrene is prepared with o-dichlorohenzene is
0.2%, the assembles concentration that the mass content of polystyrene is 1%, surplus is o-dichlorohenzene takes 10 microlitres uniformly to sprawl by liquid-transfering gun
In the prismatic silicon column template of photoetching；Silicon base is covered and is covered in the silicon column template of assembles concentration, keeps solvent equal at 80 DEG C
Even volatilization；It is cooling that withdrawing device places room temperature, re-injects 10 microlitres of CdS quantum dots by partial size 5nm, polyvinyl alcohol, and 12
The assembles concentration of sodium alkyl sulfate and water preparation, wherein CdS mass content is 0.2%, and the mass content of polyvinyl alcohol is 0.5%,
The mass content of lauryl sodium sulfate is 0.2%, and surplus is water, so that solvent is uniformly volatilized at 50 DEG C, in liquid to be assembled
After water volatilization, the micro-nano connection structure of line connecting edge form point is obtained in the silicon wafer with flat surface.
Embodiment 5
By by the CdS quantum dot of partial size 5nm, the CdS mass content that polystyrene is prepared with o-dichlorohenzene is
0.2%, the assembles concentration that the mass content of polystyrene is 1%, surplus is o-dichlorohenzene takes 10 microlitres uniformly to sprawl by liquid-transfering gun
In the star silicon column template of photoetching；Silicon base is covered and is covered in the silicon column template of assembles concentration, keeps solvent equal at 80 DEG C
Even volatilization；It is cooling that withdrawing device places room temperature, re-injects 10 microlitres of CdS quantum dots by partial size 5nm, polyvinyl alcohol, and 12
The assembles concentration of sodium alkyl sulfate and water preparation, wherein CdS mass content is 0.2%, and the mass content of polyvinyl alcohol is 0.5%,
The mass content of lauryl sodium sulfate is 0.2%, and surplus is water, so that solvent is uniformly volatilized at 50 DEG C, in liquid to be assembled
After water volatilization, the micro-nano connection structure of line connection star point is obtained in the silicon wafer with flat surface.
Embodiment 6
(wherein, the quality of polyaniline contains the saturation polyaniline assembles concentration that will be prepared by polyaniline, methyl pyrrolidone
Amount is 0.5%), to take 10 microlitres uniformly to spread in the round silicon column template of photoetching by liquid-transfering gun；Silicon base is covered and is covered with
In the silicon column template of assembles concentration, solvent is made uniformly to volatilize at 80 DEG C；Withdrawing device places room temperature cooling, re-injects 10 microlitres
The mass content for the silver nano-grain prepared by the Nano silver grain of partial size 30nm, lauryl sodium sulfate and water is
10%, the assembles concentration containing Nano silver grain that the mass content of lauryl sodium sulfate is 0.2%, surplus is water, makes solvent
It uniformly volatilizees at 50 DEG C, after the water volatilization in liquid to be assembled, obtains line connection circular dot in the silicon wafer with flat surface
Micro-nano connection structure.
Embodiment 7
By by the CdS quantum dot of partial size 5nm, the CdS mass content that polystyrene is prepared with o-dichlorohenzene is
0.2%, the assembles concentration that the mass content of polystyrene is 1%, surplus is o-dichlorohenzene takes 10 microlitres uniformly to sprawl by liquid-transfering gun
In the star silicon column template of photoetching；Silicon base is covered and is covered in the silicon column template of assembles concentration, keeps solvent equal at 80 DEG C
Even volatilization；Withdrawing device places room temperature cooling, re-injects the polystyrene sphere, 12 that 10 microlitres are about 180nm by partial size
The polystyrene sphere mass content that sodium alkyl sulfate is prepared with water is 1%, the mass content of lauryl sodium sulfate is
0.2%, surplus is the assembles concentration of water, and solvent is made uniformly to volatilize at 50 DEG C, after the water volatilization in liquid to be assembled, with smooth
The silicon wafer on surface obtains the micro-nano connection structure of line connection circular dot.
Claims (11)
1. a kind of printing process of micro-nano heterojunction structure, includes the following steps:
1) organic phase nanomaterial assembly liquid is uniformly spread over into silicon column template surface, substrate is then covered into the silicon column mould
On plate, so that the solvent in the organic phase nanomaterial assembly liquid is volatilized, just form regularly arranged receive on the substrate
The dot matrix array structure of rice material deposition；
2) water phase nanomaterial assembly liquid is injected into step 1) treated in silicon column template, make the water phase nano material group
The water volatilization in liquid is filled, nano material is just deposited in the substrate with regular linear array structure, finally in the base
The micro-nano heterojunction structure of dotted line connection is formed on bottom.
2. printing process according to claim 1, it is characterised in that: the organic phase nanomaterial assembly liquid is by nanometer
Material and organic solvent composition, wherein the mass content of the nano material is 0.01%~10%；
The water phase nanomaterial assembly liquid is made of nano material, surfactant and water, wherein the matter of the nano material
Measuring content is 0.01%~10%, and the mass content of surfactant is 0.005%~1%.
3. printing process according to claim 2, it is characterised in that: described in the organic phase nanomaterial assembly liquid
The mass content of nano material is 0.1%~1%；
The mass content of nano material described in the water phase nanomaterial assembly liquid is 0.1%~1%, the matter of surfactant
Measuring content is 0.1%~0.5%.
4. printing process according to claim 2, it is characterised in that: described in the organic phase nanomaterial assembly liquid
The particle size range of nano material described in nano material and the water phase nanomaterial assembly liquid is 2nm~900nm.
5. the printing process according to any one of claim 2-4, it is characterised in that: the organic phase nanomaterial assembly
Nano material in liquid is selected from one or more of polymer, quantum dot, organic fluorescence molecule and function small molecule；
Nano material in the water phase nanomaterial assembly liquid be selected from colloid micro ball, nano particle, carbon nanotube, graphene and
One or more of polymer.
6. the printing process according to any one of claim 2-4, it is characterised in that: the surfactant be selected from yin from
At least one of sub- surfactant, zwitterionic surfactant and nonionic surfactant.
7. the printing process according to any one of claim 2-4, it is characterised in that: the organic solvent is selected from toluene,
O-dichlorohenzene, chlorobenzene, dimethylbenzene, dimethylformamide, carbon tetrachloride, octane, heptane, n-hexane, petroleum ether and methylpyrrole
At least one of alkanone.
8. printing process according to claim 1, it is characterised in that: the substrate be selected from silicon wafer, sheet glass, quartz plate,
Any one in iron plate, copper sheet, PDMS film, PET film, PS film, PU film, PI film, aluminium flake and alumina wafer.
9. printing process according to claim 1, it is characterised in that: the micro-nano heterojunction structure of dotted line connection is respectively
The array structure of line crossing point, the array structure of line cladding point or line are by an array structure for partition.
10. printing process according to claim 1, it is characterised in that: the dot matrix array structure is according to silicon column template
Design, forms the depositing array of the similar silicon column pattern with certain altitude；
The linear array structure is to form the depositing array with certain length according to the design of silicon column template.
11. the micro-nano heterojunction structure that the described in any item printing processes of claim 1-10 are prepared.
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| CN115367697A (en) * | 2022-09-05 | 2022-11-22 | 北京仿生界面科学未来技术研究院 | Method for preparing laminated heterostructure array in patterning mode |
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