CN104129752A - Manufacturing method of cross-scale micro-nano folded structure - Google Patents
Manufacturing method of cross-scale micro-nano folded structure Download PDFInfo
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- CN104129752A CN104129752A CN201410335881.2A CN201410335881A CN104129752A CN 104129752 A CN104129752 A CN 104129752A CN 201410335881 A CN201410335881 A CN 201410335881A CN 104129752 A CN104129752 A CN 104129752A
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Abstract
The invention discloses a manufacturing method of a cross-scale micro-nano folded structure. The method comprises the following steps: (1) cleaning: cleaning a monocrystalline silicon wafer, and drying the cleaned monocrystalline silicon wafer; (2) glue coating: coating the monocrystalline silicon wafer with a layer of photoresist; (3) photoetching: forming a photoresist array structure on the monocrystalline silicon wafer; (4) film coating: coating the photoresist array structure with a layer of rigid film; and (5) pyrolyzing: pyrolyzing and contracting the photoresist to form micro-nano fold on the rigid film. A carbon structure formed after pyrolysis of the photoresist and a micro-nano structure formed by the rigid film have high current conductivity and heat conductivity, can be taken as working electrodes of micro devices such as micro sensors, micro fuel cells and biochips, and can contribute to increase in the specific surface area and the working efficiency of an electrode.
Description
Technical field
The present invention relates to micro-nano manufacturing process field, be specifically related to a kind of preparation method across the micro-nano pleated structure of yardstick.
Background technology
For having the object of elastic substrates and surface rigidity membrane structure, in the time that its elastic substrates is shunk, it is wrinkling to there is flexing in surface rigidity film under compression stress effect, and this phenomenon is conventionally taken as a kind of structural failure form and treats.In recent years, research finds, by elastic substrates being applied to specific stress, its surface rigidity film can produce corresponding regular decorative pattern, and this process provides new thinking for micro nano structure processing technology.Above-mentioned process relates to the material of elastic substrates and surface rigidity film and selects, and the mode that applies of elastic substrates ess-strain.In published Research Literature, researcher generally adopts the combination of different base material and thin-film material, and different ess-strains applies mode and carries out technical study.By the adjustment of technological parameter, can control the size of fold and pattern.Research adopts the dimethyl silicone polymer (polydimethylsiloxane of plane conventionally, or polystyrene (polystyrene PDMS), PS) for fold technique is carried out in substrate, but because the pleated structure degree of depth forming is limited, the structure of preparing by said method is two-dimensional nanostructure.In order to carry out the preparation of 3-D nano, structure, underlying structure need to be micro structure array from planar extension, although PDMS and PS can be prepared into micro structure array, the now deformation of micro-structural is difficult to apply.
Meanwhile, a kind of by the manufacturing technology of conventional lithography process and the combination of photoresist pyrolytic process, carbon micro-electromechanical systems (C-MEMS) is developed rapidly.Photoresist is a kind of organic matter being made up of elements such as hydrocarbon oxygen, high-temperature baking under reducing atmosphere, can make photoresist decompose, and causes the hydrogen-oxygen element in component to be discharged with gaseous form, the final vitreous carbon structure that obtains, has good electrical and thermal conductivity and chemical inertness.C-MEMS technique has that structural design is flexible and graphics resolution is high, simple process, favorable repeatability and low cost and other advantages.But the carbon microstructure of preparing by C-MEMS has more smooth surface conventionally, its relative surface area is less, has limited its application.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of preparation method across the micro-nano pleated structure of yardstick, its shrinkage degree controllability is good, the version of pleated pattern and dimensionally stable.
The technical solution adopted for the present invention to solve the technical problems is:
Across a preparation method for the micro-nano pleated structure of yardstick, comprise the following steps:
(1), clean: by monocrystalline silicon piece with using again acetone ultrasonic cleaning after deionized water rinsing, then monocrystalline silicon piece being put into dioxysulfate water mixed liquid heats, after taking-up, by deionized water, monocrystalline silicon piece is rinsed well and dried up with gas afterwards, then be cooled to room temperature after will monocrystalline silicon piece drying;
(2), even glue: monocrystalline silicon piece is put into sol evenning machine, apply one deck photoresist at monocrystalline silicon sheet surface, then carry out drying and processing in early stage;
(3), photoetching: the monocrystalline silicon piece that surface is coated with to photoresist is put into litho machine, utilize litho machine to expose to photoresist, then use developing liquid developing, re-using deionized water rinses photoresist and monocrystalline silicon piece to dry up with gas afterwards well, the photoresist on monocrystalline silicon piece forms micrometre array structure, and described micrometre array structure is arranged and formed by multiple photoresists unit;
(4), plated film: have the monocrystalline silicon piece of micrometre array structure to put into coating machine target and surface alignment, in the plated surface last layer stiffness films of micrometre array structure;
(5), pyrolysis: will put into tube furnace with the monocrystalline silicon piece of micrometre array structure and stiffness films, tube furnace inside vacuumizes, and passes into nitrogen and will be incubated after tube furnace intensification; Then pass into again nitrogen and hydrogen, and then insulation after heating up, make photoresist generation thermal decomposition and volume contraction, thereby make the stiffness films on photoresist surface produce fold.
Further, in step (1), the time of acetone ultrasonic cleaning is 4～6min, the ratio that dioxysulfate water mixed liquid used is is 1:1～3:1 in the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is formulated, and monocrystalline silicon piece heats 5～15min in the dioxysulfate water mixed liquid of 100～120 DEG C; The temperature of monocrystalline silicon piece drying and processing is 100～140 DEG C, and the heat time is 4～6min minute, so that the water of monocrystalline silicon sheet surface remnants is dried.
Further, the photoresist applying on monocrystalline silicon piece described in step (2) is negative photoresist, sol evenning machine first rotates 40～60s with 400～600r/min, then with 1400～1600r/min rotation, 80～120s, applies on the surface of monocrystalline silicon piece the photoresist that a layer thickness is 30～60um; Early stage, drying and processing first heated 10～20min at 55～75 DEG C of temperature, then heated 50～70min at 90～100 DEG C of temperature.
Further, in step (3), photoresist exposure dose is 1～3mJ/cm
2, the time for exposure is 50～70s; After having exposed, carry out drying and processing in mid-term, mid-term, drying and processing was to heat 30～50min at 90～100 DEG C of temperature; The developing liquid developing time is 4～6min; Then after drying up with gas, carry out later stage drying and processing, later stage drying and processing is to dry 4～6min at the temperature of 90～100 DEG C, and the micrometre array structure of formation is to be arranged and formed by the photoresist unit of multiple cylindricalitys.
Further, in step (4), have the monocrystalline silicon piece of micrometre array structure to put into respectively after the corresponding station of coating machine target and surface alignment, coating machine inside vacuumizes, and makes vacuum reach 6 × 10
-3～10 × 10
-3pa; After this in coating machine, pass into inert gas with 90～110sccm; After stable gas pressure, regulate electric current to 0.08～0.12A, start plated film, coating speed is 2～3nm/min, after 2～30 minutes, closes direct current, in the plated surface last layer stiffness films of monocrystalline silicon piece.
Further, the described tube furnace of step (5) is vacuum tube furnace, and the vacuum that tube furnace inside vacuumizes is 4 × 10
3～6 × 10
3pa; Pass into nitrogen and be raised to 250～350 DEG C with the heating rate of 5～15 DEG C/min with the flow velocity of 2000～3000sccm subsequently, and be incubated 20～40min; Then pass into nitrogen and pass into hydrogen with the flow velocity of 128～134sccm with the flow velocity of 2000～3000sccm simultaneously, be raised to 300～1000 DEG C with the heating rate of 5～15 DEG C/min, and be incubated 50～70min, photoresist is in this temperature range generation thermal decomposition and volume contraction.
Further, after photoresist pyrolysis is complete, close tube furnace, pass into nitrogen with the flow velocity of 800～1200sccm, cooling with expedite product.
As another kind of scheme of the present invention, the photoresist applying on monocrystalline silicon piece described in step (2) is positive photoresist, sol evenning machine is first with 400～600r/min rotation, 4～6s, with 1400～1600r/min rotation, 20～40s, form on the surface of monocrystalline silicon piece the photoresist that a layer thickness is 8～12um again; The temperature of carrying out drying and processing in early stage after even glue is that 100～120 DEG C of heat times are 2～4min.
Further, in step (3), the exposure dose of photoresist is 1～3mJ/cm
2the micrometre array structure forming after exposure 70～90s the 4～6min that develops is arranged and is formed by the photoresist unit of multiple cylindricalitys, in litho machine, micrometre array structure is heated to 8～12min at 120～160 DEG C more subsequently, the fusing of the photoresist unit of cylindricality refluxes and forms hemispheric photoresist unit.
Further, the ratio mixed preparing that described developer solution is 1:3～1:5 by AZ400K and deionized water by volume forms.
The invention has the beneficial effects as follows:
One, the present invention adopts the photoresist unit of micrometer structure to carry out fold technique as substrate.Photoetching process is a kind of maturation process, and good stability can carry out large area manufacture, utilizes photoresist unit that photoetching process can prepare difformity and size as substrate, therefore can capable of meeting requirements on three-dimensional fold technique prepare the requirement to underlying structure.
Two, the present invention adopts pyrolytic process to realize the contraction of substrate, after the pyrolysis of photoresist unit, forms micro-structural, and its shape and former photoresist unit are consistent substantially, and just size is corresponding dwindles.After the plated surface last layer stiffness films of photoresist unit, sample is carried out to pyrolysis, this method is easy to make the micro-structural of stiffness films to produce contraction deformation, and its shrinkage degree controllability is good, thereby the version of pleated pattern and dimensionally stable.
Three, the micro-nano structure that the micrometer structure forming after the generation pyrolysis of photoresist unit in the present invention and stiffness films form all has good conduction, thermal conductivity, the working electrode that can be used as the microdevices such as microsensor, micro fuel cell, biochip, can greatly increase the specific area of electrode and improve its operating efficiency.
Brief description of the drawings
Below in conjunction with drawings and Examples, the present invention is further detailed explanation.
Fig. 1 is the process chart of the embodiment of the present invention 1;
Fig. 2 (a), Fig. 2 (b) are respectively the present invention prepares hemispherical lithographic cell and cylindricality lithographic cell technical process schematic diagram from even glue to pyrolytic process;
Fig. 3 is the pyrolysis curve figure of embodiment 1 in the present invention;
Fig. 4 is the fold figure that in the present invention, embodiment 1 obtains;
Fig. 5 is the fold figure that in the present invention, embodiment 2 obtains;
Fig. 6 is the fold figure that in the present invention, embodiment 3 obtains;
Fig. 7 is the fold figure that in the present invention, embodiment 4 obtains.
Detailed description of the invention
Embodiment 1:
With reference to Fig. 1, Fig. 2 (b), Fig. 3 and Fig. 4, the concrete implementation step of the present embodiment is as follows:
(1) cleaning step: with carrying out acetone ultrasonic cleaning 5min after deionized water rinsing monocrystalline silicon piece (100 crystal orientation), put into again SPM solution (V after taking-up
the concentrated sulfuric acid: V
hydrogen peroxide=2:1), 110 DEG C of heating 10min, take out and rinse well by deionized water, and dry up by nitrogen gun; Finally monocrystalline silicon piece is carried out to drying and processing, at 120 DEG C, heat 5min minute, the water of monocrystalline silicon sheet surface remnants is dried, last cool to room temperature;
(2) even glue step: adopt KW-4A type sol evenning machine to carry out spin processes.On monocrystalline silicon piece, apply SU-8 negative photoresist, sol evenning machine first rotates 50s with low speed 500r/min, then with high speed 1500r/min rotation 100s, forms one deck photoresist, the thick 45um that is about of glue on the surface of monocrystalline silicon piece; The monocrystalline silicon piece that after even glue, effects on surface is covered with photoresist carries out drying and processing in early stage, heats 15min, and then heat 60min at 65 DEG C at 95 DEG C.
(3) lithography step: litho machine model used is Karl Suss MA6, and glue exposure dose is 2mJ/cm
2.SU-8 negative photoresist exposure 60s, subsequently mid-term drying and processing, at 95 DEG C, heat 40min.Use corresponding developing liquid developing 5min, use afterwards deionized water rinsing, dry up with nitrogen, the photoresist on monocrystalline silicon piece forms micrometre array structure, and described micrometre array structure is arranged and formed by multiple photoresists unit.Carry out again subsequently later stage drying and processing, at 95 DEG C, heat 5min.
The technological parameter of each step is as shown in table 1 above:
Table 1 photoetching process parameter (SU-8 negative photoresist)
(4) plated film step: utilize JS550-S/3 type magnetron sputtering coater, choosing titanium is target, carry out sputter coating, detailed process is: sample and target are put into respectively to the corresponding station of coating machine, inside vacuumizes subsequently: utilize mechanical pump, make vacuum reach 3Pa, utilize subsequently molecular pump to continue to vacuumize, make vacuum reach 8 × 10
-3pa; Open subsequently proton flowmeter, pass into high-purity argon with 100sccm; After stable gas pressure, open dc switch, electric current is adjusted to 0.1A, starts plated film, and coating speed is about 2.5nm/min, after 4 minutes, closes direct current, and titanium film thickness is about 10nm; Finally close argon gas gas circuit, open vent valve, after coating machine pressure is consistent with atmospheric pressure, sample and target are taken out.
(5) pyrolysis step: utilize GSL-1400X type vacuum tube furnace, carry out high temperature pyrolysis, detailed process is: sample is put into tube furnace, and inside vacuumizes subsequently, makes vacuum reach 5 × 10
3pa; Pass into high pure nitrogen and be raised to 300 DEG C with the heating rate of 10 DEG C/min with the flow velocity of 2500 mark condition milliliter per minutes (sccm), and be incubated 30min; Then pass into high pure nitrogen and pass into high-purity hydrogen with the flow velocity of 131sccm with the flow velocity of 2500sccm simultaneously, be raised to 400 DEG C with the heating rate of 10 DEG C/min, and be incubated 60min, photoresist thermal decomposition mainly occurs in this temperature range, this process photoresist structure volume contraction is obvious, and causes surface rigidity film to produce fold; After pyrolysis is complete, pass into high pure nitrogen with the flow velocity of 1000 mark condition milliliter per minutes (sccm), can make on the one hand to keep inert atmosphere in tube furnace, on the other hand can accelerating cooling process.
In this example, the major parameter of pyrolytic process is listed in table 2.
The pyrolytic process temperature parameter of table 2 embodiment 1
| ? | Process 1 | Process 2 | Process 3 | Process 4 | Process 5 |
| State of temperature | Heat up | Constant temperature | Heat up | Constant temperature | Cooling |
| Beginning temperature (DEG C) | Room temperature | 300 | 300 | 400 | 400 |
| End temp (DEG C) | 300 | 300 | 400 | 400 | Room temperature |
| Lifting/lowering temperature speed (DEG C/min) | 10 | 0 | 10 | 0 | Naturally annealing |
| Time (min) | \ | 30 | 10 | 60 | \ |
Embodiment 2:
Step (1) cleaning of embodiment 2, (2) even glue, (3) photoetching, (5) pyrolysis are completely identical with embodiment 1, step (4) difference.
(4) plated film step: utilize JS550-S/3 type magnetron sputtering coater, choosing titanium is target, carry out sputter coating, detailed process is: sample and target are put into respectively to the corresponding station of coating machine, inside vacuumizes subsequently: utilize mechanical pump, make vacuum reach 3Pa, utilize subsequently molecular pump to continue to vacuumize, make vacuum reach 8 × 10
-3pa; Open subsequently proton flowmeter, pass into high-purity argon with the flow velocity of 100sccm; After stable gas pressure, open dc switch, electric current is adjusted to 0.1A, starts plated film, and coating speed is about 2.5nm/min, after 20 minutes, closes direct current, and titanium film thickness is about 50nm; Finally close argon gas gas circuit, open vent valve, after coating machine pressure is consistent with atmospheric pressure, sample and target are taken out.
The difference of embodiment 2 and embodiment 1 be in plated film step the plated film time increased, in embodiment 1, the plated film time is 4min, corresponding titanium film thickness 10nm; In embodiment 2, the plated film time is 20min, corresponding titanium film thickness 50nm.With reference to Fig. 5, due to the thick difference of titanium film, the height of the fold producing after pyrolysis and width increase.
Embodiment 3:
Step (1) cleaning of embodiment 3, (2) even glue, (3) photoetching, (4) plated film are completely identical with embodiment 1, step (5) difference.
(5) pyrolysis step: utilize GSL-1400X type vacuum tube furnace, carry out high temperature pyrolysis, detailed process is: sample is put into tube furnace, and inside vacuumizes subsequently, makes vacuum reach 5 × 10
3pa; Pass into high pure nitrogen and be raised to 300 DEG C with the heating rate of 10 DEG C/min with the flow velocity of 2500 mark condition milliliter per minutes (sccm), and be incubated 30min; Then pass into high pure nitrogen and pass into high-purity hydrogen with the flow velocity of 131sccm with the flow velocity of 2500sccm simultaneously, be raised to 900 DEG C with the heating rate of 10 DEG C/min, and be incubated 60min, photoresist thermal decomposition mainly occurs in this temperature range, this process photoresist structure volume contraction is obvious, and causes surface rigidity film to produce fold; After pyrolysis is complete, pass into high pure nitrogen with the flow velocity of 1000 mark condition milliliter per minutes (sccm), keep on the one hand inert atmosphere, on the one hand accelerating cooling process.
In this example, the major parameter of pyrolytic process is listed in table 3.
The pyrolytic process temperature parameter of table 3 embodiment 3
| ? | Process 1 | Process 2 | Process 3 | Process 4 | Process 5 |
| State of temperature | Heat up | Constant temperature | Heat up | Constant temperature | Cooling |
| Beginning temperature (DEG C) | Room temperature | 300 | 300 | 900 | 900 |
| End temp (DEG C) | 300 | 300 | 900 | 900 | Room temperature |
| Lifting/lowering temperature speed (DEG C/min) | 10 | 0 | 10 | 0 | Naturally annealing |
| Time (min) | \ | 30 | 60 | 60 | \ |
The difference of embodiment 3 and embodiment 1 is that in pyrolysis step, maximum temperature has increased, and in embodiment 1, pyrolysis maximum temperature is 400 DEG C; With reference to Fig. 6, in embodiment 2, pyrolysis maximum temperature is 900 DEG C.Pyrolysis temperature is higher, can make photoresist micro-structural Substrate Contraction degree larger, and the fold width producing afterwards reduces, and highly increases.
Embodiment 4:
With reference to Fig. 2 (a), step (1) cleaning of embodiment 4, (4) plated film, (5) pyrolysis are completely identical with embodiment 1, step (2), (3) difference.
(2) even glue step: adopt KW-4A type sol evenning machine to carry out spin processes.On monocrystalline silicon piece, apply AZ9260 positive photoresist, sol evenning machine first rotates 5s with low speed 500r/min, then with high speed 1500r/min rotation 30s, the thick 10um that is about of gained glue; After even glue, monocrystalline silicon piece is carried out to drying and processing in early stage, 110 DEG C of heating 3min.
(3) lithography step: litho machine model used is Karl Suss MA6, and glue exposure dose is 2mJ/cm
2.The AZ9260 80s that exposes, does not carry out oven dry in mid-term.AZ400K is mixed to (V with deionized water
aZ400K: V
water=1:4) as developer solution, AZ9260 development 5min, uses deionized water rinsing afterwards, and nitrogen dries up.Do not carry out later stage oven dry.After AZ9260 photoetching, be column construction, in litho machine, heat after 10min at 140 DEG C again, the AZ9260 positive photoresist generation hot melt of column construction, its fusing refluxes and becomes semi-spherical shape.
The technological parameter of each step is as shown in table 4 above:
Table 4 photoetching process parameter (AZ9260 photoresist)
The difference of embodiment 4 and embodiment 1 is that even glue and lithography step parameter have changed, the structure of preparing in embodiment 1 is that the array forming is arranged in the cylindrical photoresist of SU-8 unit, and the structure of preparing in embodiment 4 is that the array forming is arranged in AZ9260 hemispherical photoresist unit.With reference to Fig. 7, can find out from the contrast of the two, underlying structure adopts different materials (positive photoresist or negative photoresist), can exert an influence to the pleated pattern on stiffness films surface.
The above, be preferred embodiments of the present invention, but the present invention is not limited to above-described embodiment, as long as it reaches technique effect of the present invention with any same or similar means, within all should falling into protection scope of the present invention.
Claims (10)
1. across a preparation method for the micro-nano pleated structure of yardstick, it is characterized in that: comprise the following steps:
(1), clean: by monocrystalline silicon piece with using again acetone ultrasonic cleaning after deionized water rinsing, then monocrystalline silicon piece being put into dioxysulfate water mixed liquid heats, after taking-up, by deionized water, monocrystalline silicon piece is rinsed well and dried up with gas afterwards, then be cooled to room temperature after will monocrystalline silicon piece drying;
(2), even glue: monocrystalline silicon piece is put into sol evenning machine, apply one deck photoresist at monocrystalline silicon sheet surface, then carry out drying and processing in early stage;
(3), photoetching: the monocrystalline silicon piece that surface is coated with to photoresist is put into litho machine, utilize litho machine to expose to photoresist, then use developing liquid developing, re-using deionized water rinses photoresist and monocrystalline silicon piece to dry up with gas afterwards well, the photoresist on monocrystalline silicon piece forms micrometre array structure, and described micrometre array structure is arranged and formed by multiple photoresists unit;
(4), plated film: have the monocrystalline silicon piece of micrometre array structure to put into coating machine target and surface alignment, in the plated surface last layer stiffness films of micrometre array structure;
(5), pyrolysis: will put into tube furnace with the monocrystalline silicon piece of micrometre array structure and stiffness films, tube furnace inside vacuumizes, and passes into nitrogen and will be incubated after tube furnace intensification; Then pass into again nitrogen and hydrogen, and then insulation after heating up, make photoresist generation thermal decomposition and volume contraction, thereby make the stiffness films on photoresist surface produce fold.
2. a kind of preparation method across the micro-nano pleated structure of yardstick according to claim 1, it is characterized in that: in step (1), the time of acetone ultrasonic cleaning is 4～6min, the ratio that dioxysulfate water mixed liquid used is is 1:1～3:1 in the volume ratio of the concentrated sulfuric acid and hydrogen peroxide is formulated, and monocrystalline silicon piece heats 5～15min in the dioxysulfate water mixed liquid of 100～120 DEG C; The temperature of monocrystalline silicon piece drying and processing is 100～140 DEG C, and the heat time is 4～6min minute, so that the water of monocrystalline silicon sheet surface remnants is dried.
3. a kind of preparation method across the micro-nano pleated structure of yardstick according to claim 1, it is characterized in that: the photoresist applying on the monocrystalline silicon piece described in step (2) is negative photoresist, sol evenning machine is first with 400～600r/min rotation, 40～60s, with 1400～1600r/min rotation, 80～120s, apply on the surface of monocrystalline silicon piece the photoresist that a layer thickness is 30～60um again; Early stage, drying and processing first heated 10～20min at 55～75 DEG C of temperature, then heated 50～70min at 90～100 DEG C of temperature.
4. a kind of preparation method across the micro-nano pleated structure of yardstick according to claim 3, is characterized in that: in step (3), photoresist exposure dose is 1～3mJ/cm
2, the time for exposure is 50～70s; After having exposed, carry out drying and processing in mid-term, mid-term, drying and processing was to heat 30～50min at 90～100 DEG C of temperature; The developing liquid developing time is 4～6min; Then after drying up with gas, carry out later stage drying and processing, later stage drying and processing is to dry 4～6min at the temperature of 90～100 DEG C, and the micrometre array structure of formation is to be arranged and formed by the photoresist unit of multiple cylindricalitys.
5. according to a kind of preparation method across the micro-nano pleated structure of yardstick described in arbitrary claim in claim 1～4, it is characterized in that: in step (4), have the monocrystalline silicon piece of micrometre array structure to put into respectively after the corresponding station of coating machine target and surface alignment, coating machine inside vacuumizes, and makes vacuum reach 6 × 10
-3～10 × 10
-3pa; After this in coating machine, pass into inert gas with 90～110sccm; After stable gas pressure, regulate electric current to 0.08～0.12A, start plated film, coating speed is 2～3nm/min, after 2～30 minutes, closes direct current, in the plated surface last layer stiffness films of monocrystalline silicon piece.
6. a kind of preparation method across the micro-nano pleated structure of yardstick according to claim 5, is characterized in that: the described tube furnace of step (5) is vacuum tube furnace, and the vacuum that tube furnace inside vacuumizes is 4 × 10
3～6 × 10
3pa; Pass into nitrogen and be raised to 250～350 DEG C with the heating rate of 5～15 DEG C/min with the flow velocity of 2000～3000sccm subsequently, and be incubated 20～40min; Then pass into nitrogen and pass into hydrogen with the flow velocity of 128～134sccm with the flow velocity of 2000～3000sccm simultaneously, be raised to 300～1000 DEG C with the heating rate of 5～15 DEG C/min, and be incubated 50～70min, photoresist is in this temperature range generation thermal decomposition and volume contraction.
7. a kind of preparation method across the micro-nano pleated structure of yardstick according to claim 6, is characterized in that: after photoresist pyrolysis is complete, close tube furnace, pass into nitrogen with the flow velocity of 800～1200sccm, cooling with expedite product.
8. a kind of preparation method across the micro-nano pleated structure of yardstick according to claim 1, it is characterized in that: the photoresist applying on the monocrystalline silicon piece described in step (2) is positive photoresist, sol evenning machine is first with 400～600r/min rotation, 4～6s, with 1400～1600r/min rotation, 20～40s, form on the surface of monocrystalline silicon piece the photoresist that a layer thickness is 8～12um again; The temperature of carrying out drying and processing in early stage after even glue is that 100～120 DEG C of heat times are 2～4min.
9. a kind of preparation method across the micro-nano pleated structure of yardstick according to claim 8, is characterized in that: in step (3), the exposure dose of photoresist is 1～3mJ/cm
2the micrometre array structure forming after exposure 70～90s the 4～6min that develops is arranged and is formed by the photoresist unit of multiple cylindricalitys, in litho machine, micrometre array structure is heated to 8～12min at 120～160 DEG C more subsequently, the fusing of the photoresist unit of cylindricality refluxes and forms hemispheric photoresist unit.
10. a kind of preparation method across the micro-nano pleated structure of yardstick according to claim 9, is characterized in that: the ratio mixed preparing that described developer solution is 1:3～1:5 by AZ400K and deionized water by volume forms.
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| CN107986224A (en) * | 2017-10-26 | 2018-05-04 | 国家纳米科学中心 | Large area multilevel surface folding structure and its preparation |
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| CN109867959A (en) * | 2018-12-28 | 2019-06-11 | 北京邮电大学 | A method of fold is formed on elastomer thin film surface |
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| CN110854005A (en) * | 2019-11-22 | 2020-02-28 | 广西民族大学 | Method for manufacturing electrode with micron structure |
| CN113184802A (en) * | 2021-05-20 | 2021-07-30 | 西安交通大学 | Preparation method of stepped annular super-hydrophobic tank |
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