CN106637075A - Method for preparing micro-nano hollow structure by laser direct writing - Google Patents
Method for preparing micro-nano hollow structure by laser direct writing Download PDFInfo
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- CN106637075A CN106637075A CN201610898582.9A CN201610898582A CN106637075A CN 106637075 A CN106637075 A CN 106637075A CN 201610898582 A CN201610898582 A CN 201610898582A CN 106637075 A CN106637075 A CN 106637075A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0623—Sulfides, selenides or tellurides
- C23C14/0629—Sulfides, selenides or tellurides of zinc, cadmium or mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/36—Removing material
- B23K26/38—Removing material by boring or cutting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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Abstract
The invention provides a method for preparing a micro-nano hollow structure by laser direct writing. The method comprises the following steps: (1) selecting a substrate, and cleaning and drying the substrate; (2) plating the substrate with a layer of amorphous zinc sulfide-silicon dioxide film by the physical vapor deposition process; (3) continually plating the zinc sulfide-silicon dioxide film with a layer of polycrystalline tin film by the physical vapor deposition process; (4) plating with an uppermost layer of zinc sulfide-silicon dioxide film by the physical vapor deposition process; and (5) performing irradiation inscribing on the prepared film with laser and enabling a hollow structure to appear in the middle of the inscribed part of the film. The method has the advantages of simple and controllable process, even product size and shape, low cost, flexible revise design, good compatibility with the conventional planar technology and the like, and can be extensively applied to such fields as microfluidics, biochips and chip interconnection.
Description
Technical field
The invention belongs to material science, and in particular to a kind of employing laser direct-writing prepares the side of micro-nano hollow structure
Method, can be used for the fields such as micro-fluidic, biochip, passage interconnection.
Background technology
It is micro-nano construction prepare breakthrough progress is obtained in the past few decades, whether architectural feature yardstick or
Complexity has significant progress.The fast development of new accurate preparation method cause it is many before had no ability to what is completed
Micro-nano structure and device have realization rate.People can realize various complex outlines by planar technology, such as MEMS,
The practical devices such as Micro-flow pipe, biochip；Gray scale mask exposure technology can realize the plane works such as curved surface profile, 3D constructions
Skill is difficult to the micro-structural for completing, such as various micro-optical devices.These technical progress promote sending out for the ability of micro-nano technology
Exhibition, but micro-nano technology technology still suffers from the deficiency in some abilities, for example, be difficult to reality in the manufacture of micro-nano hollow structure
The processing of existing shield type.
There is particularly important function in micro-nano hollow duct in many fields, from biological detection, biochip, medicine
Thing is delivered to waveguide, electronic chip, microchemical analysis and synthesis, multilayer interconnection etc..Microflow control technique is even more in these years
Technology that is fast-developing and being used widely, it possesses many advantages and for example reduces reagent consumption and quickly disease can be carried out
Diagnostic analysis.In these devices, micro-nano hollow pore passage structure is all the wherein key structure of core the most.
The surface grooves for preparing micro-meter scale using laser micro-machining technology have attracted the interest of numerous researchers.From most simple
Single surface irradiation is worked into some complicated multistep process, and these researchs obtain many significant results.But these
Processing method there is also many not enough and defects, such as longer process time, complicated process equipment, multi-step it is processed
Journey all causes these method versatilities to have a greatly reduced quality.Certain methods also need to that material is immersed in solution while performing etching
Groove can be obtained.Most of all, all of the above method can only all obtain open surface grooves, then by bonding or
The subsequent steps such as person's material bonding could obtain the hollow structure of closing.Therefore, develop it is a kind of it is inexpensive, simple efficiently, have
Nanoscale, the hollow structure processing method that can directly prepare be unusual desirable.
The content of the invention
It is an object of the invention to overcome the defect of prior art, there is provided a kind of employing laser direct-writing of innovation prepares micro-nano
The method of rice hollow structure, directly obtains hollow micro-nano hollow tunnel knot by a step is only needed in multi-layer compound film
Structure, the hollow structure of micron to nanoscale is prepared such that it is able to simple and effective, can be used for micro-fluidic, biochip etc.
Multiple fields.
The purpose of the present invention realizes that is, one kind prepares micro-nano using laser direct-writing by following main technical schemes
The method of hollow structure, the method is comprised the following steps：Step 1)：Substrate is chosen, washing and drying treatment is carried out to it；
Step 2)：One layer of amorphous zinc sulphide-silica membrane is coated with using physical gas-phase deposition in substrate；
Step 3)：Continue to be coated with one layer of polycrystalline tin using physical gas-phase deposition on zinc sulphide-silica membrane
Film；
Step 4)：The superiors' zinc sulphide-silica membrane is coated with using physical gas-phase deposition, sulfuration is integrally formed
The laminated film of the sandwich structure of zinc-silica, tin and zinc sulphide-silica；And
Step 5)：Inscription is irradiated on prepared polycrystalline tin thin film using laser, in making the film of inscription part
Between there is hollow structure.
On the basis of above-mentioned main technical schemes, the present invention further comprises following attached technical scheme：
The substrate is glass material substrate, monocrystal chip or high molecular polymer substrate, can be hard substrate, it is also possible to
It is flexible substrate.
The glass material substrate includes common cover glass, slide or quartz glass；The monocrystal chip includes monocrystalline
Silicon chip, GaAs substrate or gallium nitride substrate；
The high molecular polymer substrate is the flexible substrate of isolation material, and it includes polymethyl methacrylate
Or Merlon (PC) substrate (PMMA).
The step 2), step 4) in physical gas-phase deposition be magnetically controlled DC sputtering or rf magnetron sputtering or
Ion sputtering or pulsed laser deposition or electron beam deposition.The thickness of the film is preferably 20nm-500nm.
The step 3) in physical gas-phase deposition be that magnetically controlled DC sputtering or rf magnetron sputtering or ion splash
Penetrate or pulsed laser deposition or electron beam deposition.The thickness of the film is preferably 10nm-100nm.
The characteristic size of the hollow structure is from nanoscale to micro-meter scale；
The thickness of the amorphous zinc sulphide-silica membrane is 20nm-1000nm, and the thickness of polycrystalline tin thin film is 5nm-
200nm。
In addition, present invention also offers it is a kind of by said method prepare employing laser direct-writing prepare it is micro-nano hollow
Structure, it is characterised in that it includes：Substrate, the amorphous zinc sulphide-silica membrane being coated with using physical gas-phase deposition,
The polycrystalline tin thin film that is coated with using physical gas-phase deposition on zinc sulphide-silica membrane, positioned at the sulfuration of the superiors
Zinc-silica membrane, and it is scribed at the hollow structure that intermediate layer tin thin film is formed through laser irradiation.With prior art
Compare, the present invention has advantages below：
Using the method for the physical vapour deposition (PVD) commonly used in industrialized production preparing film, with prepare it is simple and convenient,
The advantages of pollution-free, film thickness is uniform, surface is smooth.When film thickness is 50 nanometers, about 5 nanometers of surface roughness.
2) complex steps such as need not be exposed, etch in whole preparation technology.It is by simple adjusting process parameter
The controllable micro-nano-scale hollow structure of area, thickness, size can be prepared, can be used for micro-fluidic, biochip, passage interconnection etc.
Field.
3) the inventive method production procedure cycle is short, low cost, yield is high, and process is simple is controllable, it is easy to accomplish industrialization
Production.The micro-nano-scale hollow structure of products obtained therefrom can be in fields such as micro-fluidic, biochip, the interconnections of microelectronic chip passage
There is extremely wide application prospect.
Description of the drawings
The invention will be further described to combine the embodiment of the present invention referring to the drawings, wherein：
Fig. 1 is prelaser operating diagram of the invention；
Fig. 2 is the structure chart after laser irradiation of the present invention；
Fig. 3 is the zinc sulphide-silica/tin/zinc sulphide-silica sandwich prepared according to the embodiment of the present invention one
Transmission electron microscope (TEM) image of structure composite film
Fig. 4 is the zinc sulphide-silica/tin/zinc sulphide-silica sandwich prepared according to the embodiment of the present invention two
High resolution TEM (HRTEM) image of polycrystalline tin layers in structure composite film
Fig. 5 is that the nanoscale hollow structure SEM for preparing is irradiated according to the laser of the embodiment of the present invention three
(SEM) figure；
Fig. 6 is that the micro-meter scale hollow structure SEM for preparing is irradiated according to the laser of the embodiment of the present invention four
(SEM) figure；
Fig. 7 is that the micro-meter scale hollow structure optical microscope for preparing is irradiated according to the laser of the embodiment of the present invention four (instead
Emission mode)；
Fig. 8 is that the micro-meter scale hollow structure optical microscope for preparing is irradiated according to the laser of the embodiment of the present invention five (thoroughly
Emission mode)；
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with drawings and Examples pair
The structure and preparation method of the present invention is described in further details.
As shown in Figure 1-2, the present invention provides a kind of preparation method for possessing micro-nano-scale hollow structure, and it includes as follows
Step：
Step 1)：Substrate is chosen, washing and drying treatment is carried out to it；
Step 2)：The preparation of zinc sulphide-silica membrane：By physical gas-phase deposition, one layer of zinc sulphide of growth-
Silica noncrystal membrane；Parameter during deposition can be passed through to adjust, such as deposition power, deposition pressure and sedimentation time are in base
Thickness is obtained on bottom uniform, the controllable zinc sulphide-silica membrane of thickness.The thickness of the zinc sulphide-silica membrane
For 20nm-500nm；
Step 3)：Polycrystalline tin thin film is prepared on zinc sulphide-silica membrane：It is raw by physical gas-phase deposition
Long one layer of polycrystalline tin thin film；Parameter during deposition can be passed through to adjust, such as deposition power, deposition pressure and sedimentation time are in sulphur
Change and obtain on zinc-silica membrane the polycrystalline tin thin film that thickness is uniform, thickness is controllable.The thickness of the polycrystalline tin thin film is
10nm-100nm；
Step 4)：Prepare the superiors' zinc sulphide-silica membrane：By physical gas-phase deposition, one layer of sulphur is grown
Change zinc-silica noncrystal membrane；Parameter during deposition, such as deposition power, deposition pressure and sedimentation time can be passed through to adjust
Deng obtaining in substrate, thickness is uniform, the controllable zinc sulphide-silica membrane of thickness.Zinc sulphide-the silica membrane
Thickness be 20nm-500nm；
Step 5)：Hollow knot is prepared using laser on the sandwich structure laminated film obtained by above-mentioned steps
Structure：Using laser direct writing equipment, appropriate energy density (scope 0.1-2J/cm is selected2) laser be irradiated to sample surfaces.Surface
Zinc sulphide-silica membrane light transmittance it is higher, it is few to laser energy absorption.And suction of the polycrystalline tin thin film in intermediate layer to light
High income, after laser irradiation, it may occur that photothermal deformation, the temperature for making polycrystalline tin thin film rises, tin thin film layer expanded by heating,
Zinc sulphide-silica membrane swells to form hollow structure upwards.
Further to describe in detail, the present invention also provides specific examples below：
Embodiment one：
Step 1)：Cover glass is chosen as substrate, is cleaned up the substrate using conventional semiconductor cleaning process, clearly
Dried up using dry gas after wash clean, in vacuum oven with a temperature of 120 DEG C -200 DEG C be dried, be cooled to room temperature after take
Go out；
Step 2)：R. f. magnetron sputtering amorphous zinc sulphide-dioxy is adopted in the cover glass substrate being processed as above
SiClx film, sedimentary condition：Background pressure 1 × 10-5Pa, sputtering power 50W, Ar flows be 25sccm, deposition pressure 0.1Pa,
Base reservoir temperature is room temperature, and sedimentation time 300s obtains zinc sulphide-silica-film thickness for 150nm；
Step 3)：R. f. magnetron sputtering polycrystalline tin thin film, deposition are adopted on bottom zinc sulphide-silica membrane
Condition：Background pressure 1 × 10-5Pa, sputtering power 30W, Ar flows are 25sccm, and deposition pressure 0.1Pa, base reservoir temperature is room
Temperature, sedimentation time 90s obtains polycrystalline tin thin film thickness for 10nm；
Step 4)：R. f. magnetron sputtering amorphous zinc sulphide-silica membrane, deposition are adopted on polycrystalline tin thin film
Condition：Background pressure 1 × 10-5Pa, sputtering power 50W, Ar flows are 25sccm, and deposition pressure 0.1Pa, base reservoir temperature is room
Temperature, sedimentation time 200s obtains zinc sulphide-silica-film thickness for 100nm.Above-mentioned three-layer thin-film constitutes sandwich structure
Laminated film, is made up of bottom and upper strata zinc sulphide-silica membrane and intermediate layer polycrystalline tin thin film, its cross-section structure transmission
Electronic Speculum (TEM) data are as shown in Figure 3；
Step 5)：Hollow structure is prepared using laser on the sandwich structure laminated film：Using laser direct writing equipment,
Appropriate energy density is selected (to be 1.2J/cm in the present embodiment2) laser be irradiated on sample.It is middle after laser irradiation
The temperature of layer polycrystalline tin thin film rises, and tin thin film layer expanded by heating, zinc sulphide-silica membrane swells to form hollow knot upwards
Structure.Complex thin film structure schematic diagram before and after formation hollow structure is respectively as depicted in figs. 1 and 2.
Embodiment two：
Step 1)：Choose SiO2As substrate, the substrate is cleaned up using conventional semiconductor cleaning process, cleaned
Dried up using dry gas after clean, with taking-up after being dried at a temperature of 120 DEG C -200 DEG C, being cooled to room temperature in vacuum oven；
Step 2)：In the SiO being processed as above2Deposited By Dc Magnetron Sputtering amorphous zinc sulphide-titanium dioxide is adopted in substrate
Silicon thin film, sedimentary condition：Background pressure 1 × 10-5Pa, sputtering power 80W, Ar flows be 25sccm, deposition pressure 0.08Pa, base
Bottom temperature is room temperature, and sedimentation time 400s obtains zinc sulphide-silica-film thickness for 100nm；
Step 3)：Deposited By Dc Magnetron Sputtering polycrystalline tin thin film, deposition are adopted on bottom zinc sulphide-silica membrane
Condition：Background pressure 1 × 10-5Pa, sputtering power 30W, Ar flows are 25sccm, and deposition pressure 0.08Pa, base reservoir temperature is room
Temperature, sedimentation time 100s obtains polycrystalline tin thin film thickness for 15nm；
Step 4)：Deposited By Dc Magnetron Sputtering amorphous zinc sulphide-silica membrane, deposition are adopted on polycrystalline tin thin film
Condition：Background pressure 1 × 10-5Pa, sputtering power 80W, Ar flows are 25sccm, and deposition pressure 0.08Pa, base reservoir temperature is room
Temperature, sedimentation time 400s obtains zinc sulphide-silica-film thickness for 100nm.Above-mentioned three-layer thin-film constitutes sandwich structure
Laminated film, is made up of bottom and upper strata zinc sulphide-silica membrane and intermediate layer polycrystalline tin thin film；
Step 5)：Hollow structure is prepared using laser on the sandwich structure laminated film：Using laser direct writing equipment,
(the present embodiment is 1.0J/cm to select appropriate energy density2) laser be irradiated on sample.After laser irradiation, intermediate layer
The temperature of polycrystalline tin thin film rises, and tin thin film layer expanded by heating, zinc sulphide-silica membrane swells to form hollow knot upwards
Structure.
Embodiment three：
Step 1)：Monocrystalline silicon piece is chosen as substrate, is cleaned up the substrate using conventional semiconductor cleaning process,
Dried up using dry gas after cleaning up, in vacuum oven with a temperature of 120 DEG C -200 DEG C be dried, be cooled to room temperature after take
Go out；
Step 2)：Electron beam evaporation plating deposited amorphous zinc sulphide-silica is adopted in the silicon chip substrate being processed as above
Film, sedimentary condition：Background pressure 4 × 10-5Pa, deposition power 30W, base reservoir temperature is room temperature, and sedimentation time 200s obtains sulphur
Change zinc-silica-film thickness is 100nm；
Step 3)：Deposited By Dc Magnetron Sputtering polycrystalline tin thin film, deposition are adopted on bottom zinc sulphide-silica membrane
Condition：Background pressure 1 × 10-5Pa, sputtering power 30W, Ar flows are 25sccm, and deposition pressure 0.08Pa, base reservoir temperature is room
Temperature, sedimentation time 100s obtains polycrystalline tin thin film thickness for 15nm.High resolution TEM (HRTEM) picture of its crystal grain
As shown in figure 4, finding to meet the crystal lattice data of β-Sn by measuring crystal face analysis；
Step 4)：Electron beam evaporation plating deposited amorphous zinc sulphide-silica membrane is adopted on polycrystalline tin thin film, bar is deposited
Part：Background pressure 4 × 10-5Pa, deposition power 30W, base reservoir temperature is room temperature, and sedimentation time 300s obtains zinc sulphide-titanium dioxide
Silicon film thickness is 150nm.Above-mentioned three-layer thin-film constitutes sandwich structure laminated film, by bottom and upper strata zinc sulphide-dioxy
SiClx film and intermediate layer polycrystalline tin thin film composition；
Step 5)：Hollow structure is prepared using laser on the sandwich structure laminated film：Using laser direct writing equipment,
Appropriate energy density is selected (to be 0.8J/cm in present case2) laser be irradiated on sample.After laser irradiation, intermediate layer
The temperature of polycrystalline tin thin film rises, and tin thin film layer expanded by heating, zinc sulphide-silica membrane swells to form hollow knot upwards
Structure.
Example IV：
Step 1)：Polycarbonate substrate is chosen as substrate, is cleaned the substrate using conventional semiconductor cleaning process
Totally, dried up using dry gas after cleaning up, in vacuum oven with a temperature of 60 DEG C be dried, be cooled to room temperature after take
Go out；
Step 2)：Deposited By Dc Magnetron Sputtering amorphous zinc sulphide-two is adopted on the polycarbonate substrate being processed as above
Silicon oxide film, sedimentary condition：Background pressure 1 × 10-5Pa, sputtering power 80W, Ar flows be 25sccm, deposition pressure
0.08Pa, base reservoir temperature is room temperature, and sedimentation time 400s obtains zinc sulphide-silica-film thickness for 100nm；
Step 3)：Deposited By Dc Magnetron Sputtering polycrystalline tin thin film, deposition are adopted on bottom zinc sulphide-silica membrane
Condition：Background pressure 1 × 10-5Pa, sputtering power 30W, Ar flows are 25sccm, and deposition pressure 0.08Pa, base reservoir temperature is room
Temperature, sedimentation time 200s obtains polycrystalline tin thin film thickness for 30nm；
Step 4)：Deposited By Dc Magnetron Sputtering amorphous zinc sulphide-silica membrane, deposition are adopted on polycrystalline tin thin film
Condition：Background pressure 1 × 10-5Pa, sputtering power 80W, Ar flows are 25sccm, and deposition pressure 0.08Pa, base reservoir temperature is room
Temperature, sedimentation time 800s obtains zinc sulphide-silica-film thickness for 200nm.Above-mentioned three-layer thin-film constitutes sandwich structure
Laminated film, is made up of bottom and upper strata zinc sulphide-silica membrane and intermediate layer polycrystalline tin thin film；
Step 5)：Hollow structure is prepared using laser on the sandwich structure laminated film：Using laser direct writing equipment,
Appropriate energy density is selected (to be 1.2J/cm in present case2) laser be irradiated on sample.After laser irradiation, intermediate layer
The temperature of polycrystalline tin thin film rises, and tin thin film layer expanded by heating, zinc sulphide-silica membrane swells to form hollow knot upwards
Structure.The surface Scanning Electron microscope (SEM) of the hollow structure of formation is imaged as shown in figure 5, the little figure of upper right illustrates acquisition
Hollow structure vertical section；
Embodiment five：
Step 1)：Cover glass is chosen as substrate, is cleaned up the substrate using conventional semiconductor cleaning process, clearly
Dried up using dry gas after wash clean, in vacuum oven with a temperature of 120 DEG C -200 DEG C be dried, be cooled to room temperature after take
Go out.
Step 2)：R. f. magnetron sputtering amorphous zinc sulphide-dioxy is adopted in the cover glass substrate being processed as above
SiClx film, sedimentary condition：Background pressure 1 × 10-5Pa, sputtering power 50W, Ar flows be 25sccm, deposition pressure 0.1Pa,
Base reservoir temperature is room temperature, and sedimentation time 300s obtains zinc sulphide-silica-film thickness for 150nm；
Step 3)：R. f. magnetron sputtering polycrystalline tin thin film, deposition are adopted on bottom zinc sulphide-silica membrane
Condition：Background pressure 1 × 10-5Pa, sputtering power 30W, Ar flows are 25sccm, and deposition pressure 0.1Pa, base reservoir temperature is room
Temperature, sedimentation time 90s obtains polycrystalline tin thin film thickness for 10nm；
Step 4)：R. f. magnetron sputtering amorphous zinc sulphide-silica membrane, deposition are adopted on polycrystalline tin thin film
Condition：Background pressure 1 × 10-5Pa, sputtering power 50W, Ar flows are 25sccm, and deposition pressure 0.1Pa, base reservoir temperature is room
Temperature, sedimentation time 300s obtains zinc sulphide-silica-film thickness for 150nm.Above-mentioned three-layer thin-film constitutes sandwich structure
Laminated film, is made up of bottom and upper strata zinc sulphide-silica membrane and intermediate layer polycrystalline tin thin film, its cross-section structure transmission
Electronic Speculum (TEM) data are as shown in Figure 3；
Step 5)：Hollow structure is prepared using laser on the sandwich structure laminated film：Using laser direct writing equipment,
Appropriate energy density is selected (to be 0.6J/cm in present case2) laser be irradiated on sample.After laser irradiation, intermediate layer
The temperature of polycrystalline tin thin film rises, and tin thin film layer expanded by heating, zinc sulphide-silica membrane swells to form micro-meter scale upwards
Hollow structure.The complex thin film structure SEM schematic diagrames for forming hollow structure are as shown in Figure 6.Fig. 7 illustrates the micro-fluidic of acquisition
The optical microscope picture of structure, pattern is reflective-mode.
Embodiment six：
Step 1)：Cover glass is chosen as substrate, is cleaned up the substrate using conventional semiconductor cleaning process, clearly
Dried up using dry gas after wash clean, in vacuum oven with a temperature of 120 DEG C -200 DEG C be dried, be cooled to room temperature after take
Go out；
Step 2)：R. f. magnetron sputtering amorphous zinc sulphide-dioxy is adopted in the cover glass substrate being processed as above
SiClx film, sedimentary condition：Background pressure 1 × 10-5Pa, sputtering power 50W, Ar flows be 25sccm, deposition pressure 0.1Pa,
Base reservoir temperature is room temperature, and sedimentation time 300s obtains zinc sulphide-silica-film thickness for 150nm；
Step 3)：R. f. magnetron sputtering polycrystalline tin thin film, deposition are adopted on bottom zinc sulphide-silica membrane
Condition：Background pressure 1 × 10-5Pa, sputtering power 30W, Ar flows are 25sccm, and deposition pressure 0.1Pa, base reservoir temperature is room
Temperature, sedimentation time 270s obtains polycrystalline tin thin film thickness for 30nm；
Step 4)：R. f. magnetron sputtering amorphous zinc sulphide-silica membrane, deposition are adopted on polycrystalline tin thin film
Condition：Background pressure 1 × 10-5Pa, sputtering power 50W, Ar flows are 25sccm, and deposition pressure 0.1Pa, base reservoir temperature is room
Temperature, sedimentation time 300s obtains zinc sulphide-silica-film thickness for 150nm；Above-mentioned three-layer thin-film constitutes sandwich structure
Laminated film, is made up of bottom and upper strata zinc sulphide-silica membrane and intermediate layer polycrystalline tin thin film, its cross-section structure transmission
Electronic Speculum (TEM) data are as shown in Figure 3；
Step 5)：Hollow structure is prepared using laser on the sandwich structure laminated film：Using laser direct writing equipment,
Appropriate energy density is selected (to be 0.8J/cm in present case2) laser be irradiated on sample.After laser irradiation, intermediate layer
The temperature of polycrystalline tin thin film rises, and tin thin film layer expanded by heating, zinc sulphide-silica membrane swells to form micro-meter scale upwards
Hollow structure.Fig. 8 illustrates the optical microscope picture of the hollow interconnecting electrode structure of acquisition, and pattern is transmission mode.
In the above-described embodiments, the cleaning process of substrate is conventional cleaning means, and this is easy to those skilled in the art
In what is understood, and vacuum drying purpose is to remove the hydrone remained on the substrate after cleaning.Using physical vapour deposition (PVD)
The preparation method that method prepares amorphous, polycrystal film has been known in the art, thus those of ordinary skill in the art, it will be observed that
Sedimentary condition mentioned in above-described embodiment, such as sputtering power, pressure, gas flow etc. are not unalterable.System
The method of standby film is also not necessarily limited to magnetron sputtering, electron beam evaporation plating, it is also possible to other sedimentations such as ion sputtering, as long as can make
The object of the invention is can be achieved with for corresponding amorphous, polycrystalline state film is gone out.In other embodiments of the invention, substrate is not limited to
The hard substrate such as substrate of glass, quartz, Si, PC, or flexible substrates, can equally realize the object of the invention.
Although making specific descriptions to the present invention with reference to the above embodiments, for the ordinary skill people of this area
For member, it should be appreciated that can be carried out based on present disclosure within the spirit and scope without departing from the present invention
Modification or improvement are also all within the spirit and scope of the present invention.
Claims (9)
1. a kind of method that employing laser direct-writing prepares micro-nano hollow structure, it is comprised the following steps：
Step 1)：Substrate is chosen, washing and drying treatment is carried out to it；
Step 2)：One layer of amorphous zinc sulphide-silica membrane is coated with using physical gas-phase deposition in substrate；
Step 3)：Continue to be coated with one layer of polycrystalline tin thin film using physical gas-phase deposition on zinc sulphide-silica membrane；
Step 4)：The superiors' zinc sulphide-silica membrane is coated with using physical gas-phase deposition, be integrally formed zinc sulphide-
The laminated film of the sandwich structure of silica, tin and zinc sulphide-silica；
Step 5)：Inscription is irradiated on prepared polycrystalline tin thin film using laser, is gone out in the middle of the film for making inscription part
Existing hollow structure.
2. method according to claim 1, it is characterised in that the step 5) include：Using laser direct-writing to needing system
The laminated film position of standby micro-nano hollow structure carries out direct write.
3. method according to claim 1, it is characterised in that the substrate is glass material substrate, monocrystal chip or height
Molecularly Imprinted Polymer, and substrate is hard or soft substrate.
4. method according to claim 3, it is characterised in that the glass material substrate includes common cover glass, carries glass
Piece or quartz glass；The monocrystal chip includes monocrystalline silicon piece, GaAs substrate, gallium nitride substrate.
5. method according to claim 3, it is characterised in that the high molecular polymer substrate for isolation material flexibility
Substrate, it includes polymethyl methacrylate (PMMA) or Merlon (PC) substrate.
6. method according to claim 1, it is characterised in that the step 3), in physical gas-phase deposition be magnetic
Control sputtering, ion sputtering, pulsed laser deposition or electron beam deposition.
7. method according to claim 1, it is characterised in that the characteristic size of the hollow structure is from nanoscale to micro-
Metrical scale.
8. method according to claim 1, it is characterised in that the thickness of the amorphous zinc sulphide-silica membrane is
20nm-1000nm, the thickness of polycrystalline tin thin film is 5nm-200 nm.
9. the micro-nano hollow knot that prepared by a kind of employing laser direct-writing according to the preparation of any one of claim 1-8 methods described
Structure, it is characterised in that it includes：Substrate, the amorphous zinc sulphide-silica membrane being coated with using physical gas-phase deposition,
The polycrystalline tin thin film that is coated with using physical gas-phase deposition on zinc sulphide-silica membrane, positioned at the superiors zinc sulphide-
Silica membrane, and it is scribed at the hollow structure that intermediate layer tin thin film is formed through laser irradiation.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011058A (en) * | 2012-12-13 | 2013-04-03 | 中国科学院物理研究所 | Method for preparing three-dimensional hollow micro nanometer functional structure by utilizing laser direct writing |
| CN104846348A (en) * | 2015-04-24 | 2015-08-19 | 苏州华维纳纳米科技有限公司 | Method for making microcircuit through using laser direct writing |
| CN105261671A (en) * | 2015-09-08 | 2016-01-20 | 苏州华维纳纳米科技有限公司 | Method for preparing thin-film antireflection structure employing laser direct writing |
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2016
- 2016-10-14 CN CN201610898582.9A patent/CN106637075A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103011058A (en) * | 2012-12-13 | 2013-04-03 | 中国科学院物理研究所 | Method for preparing three-dimensional hollow micro nanometer functional structure by utilizing laser direct writing |
| CN104846348A (en) * | 2015-04-24 | 2015-08-19 | 苏州华维纳纳米科技有限公司 | Method for making microcircuit through using laser direct writing |
| CN105261671A (en) * | 2015-09-08 | 2016-01-20 | 苏州华维纳纳米科技有限公司 | Method for preparing thin-film antireflection structure employing laser direct writing |
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