CN104181770B - It is a kind of that the method that micro-nano compound structure is manufactured with nano impression is printed based on 4D - Google Patents
It is a kind of that the method that micro-nano compound structure is manufactured with nano impression is printed based on 4D Download PDFInfo
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- CN104181770B CN104181770B CN201410459117.6A CN201410459117A CN104181770B CN 104181770 B CN104181770 B CN 104181770B CN 201410459117 A CN201410459117 A CN 201410459117A CN 104181770 B CN104181770 B CN 104181770B
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Abstract
The invention discloses a kind of method for being printed based on 4D and micro-nano compound structure being manufactured with nano impression, comprise the following steps：(1) micro-structural is produced by the micro-structural transfer replication on mould to impression materials using nano-imprint process；(2) it is imprinted on selective dump in micro-structural using EFI and deposits self-assembled material；(3) self-assembled material is made to occur microphase-separated, self assembly goes out micro-nano structure；(4) by micro-nano structure transfer replication to target material.Present invention incorporates the advantage of the technologies such as nano impression, increasing material manufacturing, EFI print, self assembly, the efficient of large area micro-nano composite construction, low-coat scaleization manufacture are realized, with controllability, the distinguishing feature that repeatable and uniformity is good, precision is high.
Description
Technical field
Printed and nano impression the invention belongs to minute manufacturing and increases material manufacturing technology field, more particularly to a kind of 4D that is based on
The method for manufacturing micro-nano compound structure.
Background technology
Micro-nano compound structure is the very important functional structure of nature (super-hydrophobic, gecko the strong absorption of such as lotus leaf, moth
The excellent antireflective of eye and antireflective properties useful etc.), with purposes widely.For example, lotus leaf structure have it is excellent it is super-hydrophobic,
Self-cleaning performance.The surface attachment that " lotus leaf effect " is mostly derived from the micro-nano compound structure of lotus leaf surface, i.e. lotus leaf is countless micro-
The wax mastoid process structure (5-9 microns of average diameter) of meter level, has many diameters 120 to receive in the surface distributed of each micron order mastoid process
The down-like structure of rice.The lotus leaf that the waxy substance of the special micro-nano compound structure of lotus leaf surface and low-surface-energy makes has excellent
Super-hydrophobic and self-cleaning performance.Utilize " lotus leaf effect ", be used widely in fields such as weaving, material, building, glass.Wall
The micro-nano compound structure that brave sole structure is made up of micron order bristle and nanoscale domain hair, i.e. each sole of gecko are about
500000 bristles, 30-130 μm of length, 5-10 μm of diameter；There is 400-1000 root fine hair at the top of every bristle, 2-50 μm of length, directly
Footpath 100-200nm；This micro-nano compound structure is to ensure that gecko can produce huge adhesion and adapt to different surface morphology again
Key.Gecko sole micro-nano compound structure is in MEMS and the field such as some climbing robots has boundless
Using.In silica-based solar photovoltaic cell, one layer of moth ocular structure is prepared in silicon substrate surface, reflection loss can be reduced to by 33%
Less than 3%, the efficiency of light energy utilization of battery is greatly improved, but also with self-cleaning function.In addition, aobvious in high-resolution flat board
Show, the field such as TV, mobile phone introduces function film and coating with moth ocular structure can realize that high definition is shown, Sharp Corp is
Through developing high definition moth eye TV.
Although micro-nano compound structure has a huge wide industrial applications prospect, but current facing challenges problem
Be how to realize micro-nano structure low cost, mass manufacture, especially efficiently, the controllable manufacture large area of low-coat scaleization it is micro-
Nano compound structure is always the technical barrier that domestic and international industrial circle and academia urgently break through, and has a strong impact on and restricts micro-nano and be combined
The widespread commercial application of structure.In recent years, although domestic and foreign scholars and researcher have been proposed a variety of manufacture micro-nanos and be combined
The method and strategy of structure, such as optical lithography, etching, self assembly, beamwriter lithography, focused ion beam, laser interference lithography,
Soft lithographic, nano impression etc., but they all deposit limitation in some aspects and it is not enough (such as graphical area, efficiency, into
Sheet, uniformity, precision, repeatability etc.), existing technique and solution are also difficult to meet industrialized production and application at present
It is required that.
Therefore, how inexpensive, extensive repeatable manufacture large area micro-nano composite construction is currently urgently to break through
Internationalization technical barrier.
The content of the invention
The present invention is in order to solve the above problems, it is proposed that one kind manufactures micro-nano compound structure based on 4D printings and nano impression
Method, this method combines nanometer pressure using the minute manufacturing combination process being combined " from top to bottom " and " from bottom to top "
The advantage of the technologies such as print, increasing material manufacturing, EFI print, self assembly, realizes efficient, the inexpensive rule of large area micro-nano composite construction
Modelling is manufactured, with controllability, the distinguishing feature that repeatable and uniformity is good, precision is high.
To achieve these goals, the present invention is adopted the following technical scheme that：
It is a kind of that the method that micro-nano compound structure is manufactured with nano impression is printed based on 4D, comprise the following steps：
(1) micro-structural is produced by the micro-structural transfer replication on mould to impression materials using nano-imprint process；
(2) it is imprinted on selective dump in micro-structural using EFI and deposits self-assembled material；
(3) self-assembled material is made to occur microphase-separated, self assembly goes out micro-nano structure；
(4) by micro-nano structure transfer replication to target material.
The specific method of the step (1) includes：
(1-1) applies one layer of liquid impression materials of paving in substrate；
(1-2) uses soft UV nano-imprint process, contour roll forming nano-imprint process or hot nano impression technique, by mould
Micro-structural transfer replication is on impression materials；
(1-3) removes residual layer, and micro-structural is produced on impression materials.
In the step (1-1), the substrate is non-conducting material or conductive material, when the substrate is conductive material
When, it is necessary to thereon first deposit one layer of dielectric material.
In the step (1-1), the impression materials are UV curing conductives liquid polymer or the heat with conductive characteristic
Impression materials.
In the step (1-2), the micro-structural is boss structure, and the boss structure includes but is not limited to cylinder, circle
Platform, square boss, hexagonal boss and trapezoid boss.
In the step (2), specific method includes：
Substrate with micro-structural is placed on EFI print workbench by (2-1)；
(2-2), using self-assembled material as printed material, using electric jet printing technique, selective spray printing sinks in substrate micro-structural
One layer of self-assembled material of product；Because substrate is non-conducting material, the micro-structural of impressing is conductive, EFI print injection from group
Package material, which can be oriented, selectively to be deposited in micro-structural, and self-assembled material will not be deposited in other regions.
The self-assembled material includes di-block copolymer, triblock copolymer or Tetrablock copolymer material, works as use
During di-block copolymer PS-b-PMMA, the di-block copolymer PS-b-PMMA volume fractions f is 0.6-0.8, deposit thickness
For 100-600nm.
The technological parameter that the EFI print is used：Voltage 350V-500V, height 20-30 micron of the shower nozzle apart from base material.
In the step (3), when self-assembled material is di-block copolymer PS-b-PMMA, its specific method includes：
(3-1) in a nitrogen environment, anneals 5-60 minutes at 180 DEG C~260 DEG C, di-block copolymer PS-b-PMMA hairs
Raw microphase-separated, self assembly goes out the micro-nano structure perpendicular to substrate；
(3-2) uses deep UV exposure, and dosage is 25J/cm2, the time for exposure is 2-5 minutes, identical in degraded PMMA
When crosslinking curing PS phases；
(3-3) is soaked 2-4 hours using glacial acetic acid, and dissolving removes the PMMA phases after decomposing.
In the step (4), the specific method of transfer replication micro-nano structure is：
Using PS phases template as mask, using etching technics by PS phase micro-nano structure transfer replications to micro-structural；Or with PS
Phase template is mask, using deposition, electroforming, lift-off techniques, by PS phase micro-nano structure transfer replications to functional material, is manufactured
Go out micro-nano compound structure.
The micro-nano structure includes but is not limited to nano-pillar, nano-pore and nanometer wall construction.
The micro-nano structure of the self assembly includes but is not limited to spherical phase, columnar phase, lamellar phase or helical form phase.
Beneficial effects of the present invention are：
(1) advantage of the techniques such as nano impression, increasing material manufacturing, EFI print, self assembly is combined, is a kind of " from top to bottom "
" from bottom to top " the micro-nano composite manufacturing technology being combined；
(2) the controllable manufacture large area micro-nano composite construction of efficient, inexpensive mass can be achieved；
(3) substrate is applied widely, i.e., suitable for hard substrate, is also applied for flexible substrates；
(4) have the advantages that low cost, uniformity, controllability and favorable repeatability, precision are high；
(5) realize grand and/micro-/receive across yardstick manufacture；
(6) have wide range of applications, the various bionical micro-nanos such as lotus leaf structure, gecko sole structure, moth ocular structure can be used for
Composite construction, can be used for manufacture super capacitor, micro- energy, receives the fields such as photonic device.
Brief description of the drawings
Fig. 1 is that the present invention manufactures micro-nano compound structure process route chart based on 4D printings and nano impression；
Fig. 2 a are that the present invention manufactures micro-nano compound structure embodiment schematic diagram based on 4D printings and nano impression.
Fig. 2 b are that the present invention manufactures micro-nano compound structure embodiment schematic diagram based on 4D printings and nano impression.
Fig. 2 c are that the present invention manufactures micro-nano compound structure embodiment schematic diagram based on 4D printings and nano impression.
Fig. 2 d are that the present invention manufactures micro-nano compound structure embodiment schematic diagram based on 4D printings and nano impression.
Fig. 2 e are that the present invention manufactures micro-nano compound structure embodiment schematic diagram based on 4D printings and nano impression.
Fig. 2 f are that the present invention manufactures micro-nano compound structure embodiment schematic diagram based on 4D printings and nano impression.
Fig. 2 g are that the present invention manufactures micro-nano compound structure embodiment schematic diagram based on 4D printings and nano impression.
Wherein, 1, substrate (glass)；2nd, impression materials (UV curing conductives liquid polymer or conductive characteristic hot padding material
Material)；3rd, micro-structural；4th, self-assembled material (di-block copolymer PS-b-PMMA)；401st, di-block copolymer PS phases；402 liang embedding
Section copolymer p MMA phases；5th, other regions in addition to micro-structural；6th, nano-pore；7th, forwarding function material；8th, micro-nano structure；9th, PS phases mould
Plate.
Embodiment：
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
The present invention is adopted the following technical scheme that：
(1) using nano impression manufacture micro-structural (patterned substrate)；
(2) self-assembled material di-block copolymer PS-b-PMMA selective dumps are deposited on using electric Printing techniques micro-
(realize that selective dump deposits self-assembled material with reference to patterned substrate and EFI print) in structure；
(3) make annealing treatment, self assembly micro-nano structure；
(4) crosslinking curing PS phases when using Deep Ultraviolet exposure degraded PMMA identical, then remove PMMA phase (PS phase moulds
Plate)；
(5) using etching, deposition, electroforming, the technique such as lift-off by PS phase micro-nano structure transfer replications to micro-structural or
On other functional materials, micro-nano compound structure is produced.
One kind manufactures micro-nano compound structure method based on 4D printings and nano impression, specifically includes following processing step：
(1) nano impression manufacture micro-structural；
(2) EFI print selective dump self-assembled material；
(3) self assembly micro-nano structure；
(4) transfer replication micro-nano structure.
In step (1), the specific method for manufacturing micro-structural using nano impression includes：
1. one layer of liquid impression materials of paving are applied in substrate (substrate, base material), the substrate is non-conducting material, the pressure
Print material is UV curing conductive liquid polymers；
2. soft UV nano-imprint process or contour roll forming nano-imprint process are used, the micro-structural transfer replication on mould is arrived
On impression materials, the micro-structural is boss structure, including such as cylinder, round platform, square boss, hexagonal boss, trapezoidal convex
Platform etc.；
3. residual layer is removed, micro-structural is produced on impression materials；
In step (2), it is imprinted on selective dump in micro-structural using EFI and deposits self-assembled material di-block copolymer
Specific method includes：
1. the substrate (patterned substrate) with micro-structural is placed on EFI print workbench；
2. it is micro- in substrate using electric jet printing technique using self-assembled material di-block copolymer PS-b-PMMA as printed material
Selective spray printing deposits one layer of di-block copolymer PS-b-PMMA in structure.Because substrate is non-conducting material, micro- knot of impressing
Structure is conductive (conducting polymer), and the di-block copolymer PS-b-PMMA of EFI print injection, which can be oriented, selectively to sink
Accumulate onto micro-structural, di-block copolymer PS-b-PMMA will not be deposited in other regions.The di-block copolymer PS-b-
PMMA volume fractions f is 0.6-0.8, and deposit thickness is 100-600nm.The technological parameter that the EFI print is used：Voltage 350V-
500V, height 20-30 micron of the shower nozzle apart from base material.
In step (3), the specific method of self-assembled nano structures includes：
1. in a nitrogen environment, annealed 5-60 minutes at 180 DEG C~260 DEG C, di-block copolymer PS-b-PMMA occurs micro-
It is separated, self assembly goes out the micro-nano structure perpendicular to substrate, the micro-nano structure includes nano-pillar, nano-pore, nm wall (layer structure
Phase) etc. structure；
2. deep UV exposure is used, dosage is 25J/cm2, the time for exposure is 2-5 minutes, is handed over when the PMMA that degrades is identical
Connection solidification PS phases；
3. soaked 2-4 hours using glacial acetic acid, dissolving removes the PMMA phases after decomposing.
In step (4), the specific method of transfer replication micro-nano structure includes：
Using PS phases template as mask, using etching technics by PS phase micro-nano structure transfer replications to micro-structural.Or with PS
Phase template is mask, using deposition, electroforming, lift-off techniques, by PS phase micro-nano structure transfer replications to other functional materials
(such as nickel, copper, cobalt).
If substrate is conductive material, it is necessary to first deposit one layer of dielectric material thereon.
Impression materials can also use the hot padding material with conductive characteristic, and the manufacture of corresponding micro-structural uses hot nanometer
Imprint process.
Substrate both can be hard substrate or flexible substrates.
Self-assembled material also includes other di-block copolymers, triblock copolymer, Tetrablock copolymer material.
The micro-nano structure of self assembly includes spherical phase, columnar phase, lamellar phase, helical form phase.
Embodiment one,
The present embodiment is using glass as substrate 1, and the micro-nano compound structure to be manufactured is a kind of imitative lotus leaf micro-nano compound structure,
Micro-structural 3 is a diameter of 6 microns of cylindrical-array (class mastoid process structure), and the cycle is 10 microns, 4 microns of cylinder height, micro-nano structure 8
For 120 nanometers of nano wire (class down-like structure) of diameter.Specific manufacturing technology steps are as follows：
(1) micro-structural 3 is manufactured using nano impression
1. 4.5 microns of thickness UV solidifications of paving and conductive liquid polymer impression materials 2, such as Fig. 2 a are applied in substrate of glass 1
It is shown；
2. soft UV nano-imprint process is used, by the micro-structural imprinting and copying on soft mold to polymer impression materials 2；
3. residual layer is removed using reaction and plasma etching technics, formed on the impression materials 2 on substrate of glass 1
The cylindrical-array of minute yardstick, obtains micro-structural 3, as shown in Figure 2 b.
(2) EFI print selective dump self-assembled material 4
1. the substrate 1 (patterned substrate) with micro-structural 3 step (1) manufactured is placed on EFI print workbench；
2. using self-assembled material di-block copolymer PS-b-PMMA as printed material 4 (volume fraction f is 0.7), electricity is utilized
Jet printing technique di-block copolymer PS-b- thick selective spray printing deposition 200nm in the cylindrical-array micro-structural 3 on base material
(because substrate 1 is non-conducting material, the fine structure material of impressing is conductive, and two blocks of EFI print injection are total to by PMMA 4
Polymers PS-b-PMMA4 can directional selectivity deposit in cylindrical-array micro-structural 3, other regions 5 beyond micro-structural
(non-conductive substrate regions) do not have di-block copolymer PS-b-PMMA4) deposition, as shown in Figure 2 c.The work that EFI print is used
Skill parameter：Voltage 400V, height 30 micron of the shower nozzle apart from base material.
(3) self assembly micro-nano structure 8
1. the substrate 1 that deposition has di-block copolymer PS-b-PMMA 4 is placed in the annealing furnace full of nitrogen, 220
Annealed 5 minutes at DEG C, microphase-separated occurs for di-block copolymer PS-b-PMMA 4, self assembly obtains PMMA column microfacies and receives knot
Structure 402 (perpendicular to substrate 1), as shown in Figure 2 d；
2. deep UV exposure is used, exposure dose is 25J/cm2, the time for exposure is 2-5 minutes, in degraded PMMA phases
402 while crosslinking curing PS phases 401；
3. soaked 2-4 hours using glacial acetic acid, dissolving removes the PMMA phases 402 after decomposing, and obtains nano-pore 6, its diameter
For 120nm PS phases template 9 (nanohole array of diameter 120), as shown in Figure 2 e.
(4) transfer replication micro-nano structure
1. it is mask with PS phases template 9, metal nickel nano-line 7 is grown in nano-pore using electrodeposition process, such as Fig. 2 f institute
Show；
2. it is placed into high temperature process furnances, is passed through argon gas protection, 5 are incubated after being heated to 500 DEG C with 5 DEG C/min programming rates
Hour, after natural cooling, PS phases (polystyrene) 401 are removed, micro-nano compound structure (3,8) are obtained, as shown in Figure 2 g.
Step (4) transfer replication micro-nano structure 8, can also use etching technics, be mask with PS phases template 9, by micro-nano structure 8
Direct transfer replication obtains micro-nano compound structure (3,8) in micro-structural 3.
Although above-mentioned the embodiment of the present invention is described with reference to accompanying drawing, not to present invention protection model
The limitation enclosed, one of ordinary skill in the art should be understood that on the basis of technical scheme those skilled in the art are not
Need to pay various modifications or deform still within protection scope of the present invention that creative work can make.
Claims (11)
1. a kind of print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：Comprise the following steps：
(1) micro-structural is produced by the micro-structural transfer replication on mould to impression materials using nano-imprint process；
(2) it is imprinted on selective dump in micro-structural using EFI and deposits self-assembled material；
(3) self-assembled material is made to occur microphase-separated, self assembly goes out micro-nano structure；
(4) by micro-nano structure transfer replication to target material.
2. as claimed in claim 1 print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：Institute
Stating the specific method of step (1) includes：
(1-1) applies one layer of liquid impression materials of paving in substrate；
(1-2) uses soft UV nano-imprint process, contour roll forming nano-imprint process or hot nano impression technique, by micro- knot on mould
Structure transfer replication is on impression materials；
(1-3) removes residual layer, and micro-structural is produced on impression materials.
3. as claimed in claim 2 print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：Institute
State in step (1-1), the substrate is non-conducting material or conductive material, when the substrate is conductive material, it is necessary at it
It is upper first to deposit one layer of dielectric material.
4. as claimed in claim 2 print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：Institute
State in step (1-1), the impression materials are UV curing conductives liquid polymer or the hot padding material with conductive characteristic.
5. as claimed in claim 2 print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：Institute
State in step (1-2), the micro-structural is boss structure, the boss structure includes but is not limited to cylinder, round platform, square convex
Platform, hexagonal boss and trapezoid boss.
6. as claimed in claim 1 print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：Institute
State in step (2), specific method includes：
Substrate with micro-structural is placed on EFI print workbench by (2-1)；
(2-2), using self-assembled material as printed material, using electric jet printing technique, selective spray printing deposits one in substrate micro-structural
Layer self-assembled material；Because substrate is non-conducting material, the micro-structural of impressing is conductive, the self assembly material of EFI print injection
Material, which can be oriented, selectively to be deposited in micro-structural, and self-assembled material will not be deposited in other regions.
7. as claimed in claim 6 print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：Institute
Stating self-assembled material includes di-block copolymer, triblock copolymer or Tetrablock copolymer material, when using two block copolymerizations
During thing PS-b-PMMA, the di-block copolymer PS-b-PMMA volume fractions f is 0.6-0.8, and deposit thickness is 100-
600nm。
8. as claimed in claim 6 print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：Institute
State the technological parameter that EFI print is used：Voltage 350V-500V, height 20-30 micron of the shower nozzle apart from base material.
9. as claimed in claim 1 print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：Institute
State in step (3), when self-assembled material is di-block copolymer PS-b-PMMA, its specific method includes：
(3-1) in a nitrogen environment, anneals 5-60 minutes at 180 DEG C~260 DEG C, and di-block copolymer PS-b-PMMA occurs micro-
It is separated, self assembly goes out the micro-nano structure perpendicular to substrate；
(3-2) uses deep UV exposure, and dosage is 25J/cm2, the time for exposure is 2-5 minutes, is crosslinked when the PMMA that degrades is identical
Solidify PS phases；
(3-3) is soaked 2-4 hours using glacial acetic acid, and dissolving removes the PMMA phases after decomposing.
10. as claimed in claim 1 print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：
In the step (4), the specific method of transfer replication micro-nano structure is：
Using PS phases template as mask, using etching technics by PS phase micro-nano structure transfer replications to micro-structural；Or with PS phase moulds
Plate is mask, using deposition, electroforming, lift-off techniques, by PS phase micro-nano structure transfer replications to functional material, is produced micro-
Nano compound structure.
11. as claimed in claim 1 print the method that micro-nano compound structure is manufactured with nano impression based on 4D, it is characterized in that：
In the step (3), (4), the micro-nano structure includes but is not limited to nano-pillar, nano-pore and nanometer wall construction；The self assembly
The micro-nano structure gone out includes but is not limited to spherical phase, columnar phase, lamellar phase and helical form phase.
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| CN104690969B (en) * | 2015-02-10 | 2017-04-19 | 西安交通大学 | Bionic irregular micro nano composite structure manufacturing process based on 3D ejection printing technique |
| CN105984151A (en) * | 2016-06-21 | 2016-10-05 | 李钢 | Ship four-dimensional space-time energy-containing memory printing system |
| CN106313573A (en) * | 2016-08-31 | 2017-01-11 | 青岛理工大学 | 3D printing method for embedded electronic product |
| CN110573321B (en) * | 2017-04-25 | 2021-12-21 | 昕诺飞控股有限公司 | Imprinted 3D printing structure, printing method, 3D article and lighting system with 3D article |
| CN112219164A (en) * | 2018-03-26 | 2021-01-12 | 应用材料公司 | Method for producing a multi-layer imprint master, multi-layer imprint master and use of a multi-layer imprint master |
| EP3821456A4 (en) * | 2018-07-10 | 2022-03-16 | B.G. Negev Technologies and Applications Ltd., at Ben-Gurion University | A nanocomposite mold for thermal nanoimprinting and method for producing the same |
| CN112060568B (en) * | 2020-07-27 | 2022-01-28 | 南京大学 | Photocuring additive manufacturing method |
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