CN107814353A - The method that nanometer pinpoint array is prepared on transparent flexible substrate - Google Patents
The method that nanometer pinpoint array is prepared on transparent flexible substrate Download PDFInfo
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- CN107814353A CN107814353A CN201711020715.3A CN201711020715A CN107814353A CN 107814353 A CN107814353 A CN 107814353A CN 201711020715 A CN201711020715 A CN 201711020715A CN 107814353 A CN107814353 A CN 107814353A
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- flexible substrate
- transparent flexible
- nanometer pinpoint
- array
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00134—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems comprising flexible or deformable structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
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- Application Of Or Painting With Fluid Materials (AREA)
Abstract
The invention provides a kind of method that nanometer pinpoint array is prepared on transparent flexible substrate, realization prepares nanometer pinpoint array, prepares the characteristics of area is big, technique is simple, it is characterised in that this method comprises the following steps on flexible substrates：Step 1. prepares PS ball array templates by liquid level self assembly；Step 2. constructs nanometer pinpoint array template using the irradiation of oxygen plasma etch coupled ion beam on substrate；Step 3. spin coating PDMS on substrate of the surface with nanometer pinpoint array template, then peel off and obtain PDMS templates；Step 4. one layer of ultra-violet curing photo etching of spin coating on transparent flexible substrate, PDMS templates are pressed on transparent flexible substrate, after being solidified using uv light irradiation, are taken PDMS templates off, are obtained nanometer pinpoint array.
Description
Technical field
The invention belongs to field of nano material preparation, and in particular to nanometer pinpoint array is prepared on transparent flexible substrate
Method.
Technical background
The appearance of nanometer technology has greatly facilitated the progress of science and technology, and with the continuous progress of technology, its machining accuracy is
Reach nanoscale.Present nanofabrication technique has been widely applied to the fields such as machinery, optics, electronic information, the energy.It is main
Processing method is wanted to be divided into physics and the class of chemical method two, including photoetching, focused ion beam, nanometer embossing, scanning probe lithography
Technology etc..The nanometer pinpoint array of high-sequential causes it in photocatalysis, solar cell, light due to its special optical characteristics
The field such as electrical part and SERS suffers from important application.But it is constrained to current technology, it is desirable to obtain large area, superelevation
The nanoscale pinpoint array of the uniformity is still a challenge.Tradition prepares the method for large area array such as：Ultraviolet photolithographic and
Focused ion beam etc. has its limitation.Photoetching technique can realize the array of large area high uniformity, but be received for preparation
Meter level array is but difficult to.Although focused ion beam system can realize less than 50 nanometers of array structure, but can not be real
The preparation of existing large area.
In order to obtain large area, the nanometer pinpoint array of small size, some improved process technologies are introduced into such field.
Such as atom lithography, atom lithography can reach 0.1 nanometer due to its diffraction limit very little, therefore have high resolution ratio, but
It is that how to obtain the atom line of high intensity be a problem.And for example nano impression, nano impression can realize large area, fast
It is prepared by fast, high-precision nanostructured；But cost becomes higher when structure dimension is reduced to nanoscale.These improved sides
Method has its advantage, but still has some problem urgent need to resolve.
The content of the invention
The present invention is, and it is an object of the present invention to provide a kind of prepare on transparent flexible substrate in order to solving the above problems and carry out
The method of nanometer pinpoint array, this method can be realized prepares nanometer pinpoint array on flexible substrates, prepare area it is big,
The characteristics of technique is simple.
The present invention to achieve these goals, employs following scheme：
The present invention provides a kind of method that nanometer pinpoint array is prepared on transparent flexible substrate, it is characterised in that including
Following steps：Step 1. prepares PS ball array templates by liquid level self assembly；Step 2. using oxygen plasma etch combine from
Nanometer pinpoint array template is constructed in beamlet irradiation on substrate；Step 3. carries the substrate of nanometer pinpoint array template on surface
Upper spin coating PDMS, then peel off and obtain PDMS templates；Step 4. one layer of ultra-violet curing photo etching of spin coating on transparent flexible substrate, will
PDMS templates are pressed on transparent flexible substrate, after solidifying using uv light irradiation, are taken PDMS templates off, are obtained nanometer pinpoint battle array
Row.
Further, the method provided by the invention for preparing nanometer pinpoint array on transparent flexible substrate can also have
Following characteristics：In step 2, the ion beam used is nitrogen ion beam, irradiation energy 20keV, irradiation dose be more than or equal to 3 ×
1016ions/cm2, and less than 1 × 1017ions/cm2。
Further, the method provided by the invention for preparing nanometer pinpoint array on transparent flexible substrate can also have
Following characteristics：In step 3, the substrate that spin coating has PDMS is put into baking oven and is heated to 50~70 DEG C, and it is small to be incubated 1~2
When, strip operation is then carried out again.
Further, the method provided by the invention for preparing nanometer pinpoint array on transparent flexible substrate can also have
Following characteristics：In step 3, curing agent is mixed with PDMS, here, PDMS is the glue of SYLGARD 184, is divided into A, B glue, B glue
As solidification glue, and be A and the mass ratio of B glue is 10:1, both are mixed evenly before spin coating, and centrifuged with
Eliminate bubble.
Further, the method provided by the invention for preparing nanometer pinpoint array on transparent flexible substrate can also have
Following characteristics：In step 4, transparent flexible substrate is PET film substrate.
Further, the method provided by the invention for preparing nanometer pinpoint array on transparent flexible substrate can also have
Following characteristics：In step 4, ultra-violet curing photo etching is NOA61.
Further, the method provided by the invention for preparing nanometer pinpoint array on transparent flexible substrate can also have
Following characteristics：In step 4, the parameter of spin coating ultra-violet curing photo etching is 3000~5000 revs/min, 30~60 seconds.
Further, the method provided by the invention for preparing nanometer pinpoint array on transparent flexible substrate can also have
Following characteristics：In step 4, ultraviolet irradiation hardening time is 30 minutes.
The effect of invention and effect
The method stability provided by the invention that nanometer pinpoint array is prepared on transparent flexible substrate is high, and repeatability
Good, technique is simple, and cost is low, can effectively mark the pinpoint array for preparing wafer scale, and nanometer pinpoint size is at 50 nanometers
Left and right, area can reach 4 inch wafer levels.
Brief description of the drawings
Fig. 1 is the SEM figures that nanometer pinpoint array template procedure is prepared in the embodiment of the present invention one, wherein, (a) is PS spherical arrays
The SEM figures of row, (b) are that the SEM figures after corona treatment are carried out to PS balls, and (c) is further to carry out ion beam irradiation processing
SEM figures afterwards, (d) are the sectional view of (c)；
Fig. 2 is the image of the nanometer pinpoint array prepared in the embodiment of the present invention one using reverse stamping method on PET, its
In, (a) is photomacrograph；(b) scheme for SEM；
Fig. 3 is the AFM figures for the nanometer pinpoint array prepared in the embodiment of the present invention one, wherein, (a) is AFM three-dimensional shapeds
Looks figure, (b) are AFM two-dimensional appearance figures, and (c) is depth of section curve map；
Fig. 4 (a) is the SEM figures that nanometer pinpoint array process is prepared in the embodiment of the present invention two, wherein, (a) is to PS balls
The SEM figures after corona treatment and ion beam irradiation processing are carried out, (b) is that the SEM of nanometer pinpoint array schemes；
Fig. 5 is the AFM figures for the nanometer pinpoint array prepared in the embodiment of the present invention two, wherein, (a) is AFM three-dimensional shapeds
Looks figure, (b) are AFM two-dimensional appearance figures, and (c) is depth of section curve map；
Fig. 6 is the SEM figures that nanometer pinpoint array process is prepared in the embodiment of the present invention three, wherein, (a) is that PS balls are carried out
SEM figures after corona treatment and ion beam irradiation processing, (b) are that the SEM of nanometer pinpoint array schemes.
Embodiment
Tool below in conjunction with accompanying drawing to the method for the present invention that nanometer pinpoint array is prepared on transparent flexible substrate
Body embodiment is described in detail.
<Embodiment one>
In the present embodiment one, the method that nanometer pinpoint array is prepared in flexible substrate (PET) is broadly divided into two processes.
First process is to prepare nanometer pinpoint on a silicon substrate by the method for ion beam irradiation combination PS ball masks
Array mould plate, concrete operations are as follows：
As shown in Fig. 1 (a), the PS ball arrays of the uniform solid matter of large area are first prepared on a silicon substrate using liquid level assembling；Lining
Bottom needs to do clear water processing in advance, is typically soaked using SDS.Then, the silicon substrate for being covered with PS arrays is subjected to oxygen plasma
Processing, power 30W, time 1h, obtains the structure as shown in Fig. 1 (b), PS bulb diameters are less than 500nm after processing, are advantageous to contract
The time of short next step ion beam irradiation.Further, ion beam can also be reduced to substrate by shortening the time of ion beam irradiation
Destroy.Because heavy dose of ion beam irradiation can cause substrate surface cavity occur, the experiment after us can be thus influenceed
Process.
After oxygen plasma processing is carried out to PS ball arrays, sample is put into ion implantation apparatus and performed at ion irradiation
Reason, Implantation Energy 20keV, dosage are 5 × 1016ions/cm2, the sample SEM figures after processing are as shown in Fig. 1 (c), Fig. 1 (d)
Scheme for its corresponding section SEM.The nanometer pinpoint size obtained under this irradiation parameters is highly received 200 in 50 rans
Rice or so.
Second process is reversely marks nanometer pinpoint using reverse stamping method on PET substrate, and concrete operations are such as
Under：
First, nanometer pinpoint template is coated into PDMS, 4000 revs/min of rotating speed, 30 seconds time；PDMS needs mixing cured
Agent stirs (mass ratio PDMS:Curing agent=10:1), and using centrifuge there is no bubble into solution.
Then, sample is put into baking oven baking, temperature is 70 DEG C, and the time is 1 hour, and this process is to speed up PDMS solidifications
Form reversely marking template.After treating that PDSM is fully cured, PDMS is stripped down.It can be formed and received on the PDMS films stripped down
Metre hole array, can have template as the casting for preparing nanometer pinpoint.
Next, by spin-coating method on PET one layer of NOA61 uv-curable glue of spin coating.Need to carry out PET before spin coating
Cleaning, it is cleaned by ultrasonic respectively with acetone, ethanol, deionized water.The PDMS templates that will be stripped down after spin coating uv-curable glue
It is pressed on PET and carries out ultraviolet light irradiation 30 minutes, then peel off PDMS templates, if Fig. 2 is to be made by reversely marking on PET
Standby nanometer pinpoint array.SEM image shows that this method can realize prepared by the nanometer pinpoint of overlarge area.As shown in figure 3,
Understand the height of nanometer pinpoint in 50 rans by measurement.
<Embodiment two>
In the present embodiment two, preparation process is identical with embodiment one, and only specific experiment parameter is different：
First, the PS ball arrays of the uniform solid matter of large area are prepared on a silicon substrate using liquid level assembling；Then PS will be covered with
The silicon substrate of array carries out oxygen plasma processing, power 30W, time 1h so that PS bulb diameters are less than 500nm after processing.
After oxygen plasma processing is carried out to PS ball arrays, sample is put into ion implantation apparatus and performed at ion irradiation
Reason, Implantation Energy 20keV, dosage are 3 × 1016ions/cm2。
Then, nanometer pinpoint template is coated into PDMS, 4000 revs/min of rotating speed, 30 seconds time；PDMS needs mixing cured
Agent stirs (PDMS:Curing agent=10:1), and using centrifuge there is no bubble into solution.
Then, sample is put into baking oven baking, temperature is 70 DEG C, and the time is 1 hour., will after treating that PDSM is fully cured
PDMS is stripped down.Nanohole array can be formed on the PDMS films stripped down, can have mould as the casting for preparing nanometer pinpoint
Plate.
Next, by spin-coating method on PET one layer of NOA61 uv-curable glue of spin coating.Need to carry out PET before spin coating
Cleaning, it is cleaned by ultrasonic respectively with acetone, ethanol, deionized water.The PDMS templates that will be stripped down after spin coating uv-curable glue
It is pressed on PET and carries out ultraviolet light irradiation 30 minutes, then peels off PDMS templates.It can be found that after template size increases, reversely
Mark obtained array sizes and also correspond to increase, as shown in figure 5, tip diameter is highly 180nm to of about 240nm.
<Embodiment three>
In the present embodiment three, preparation process is identical with embodiment one, and only specific experiment parameter is different：
First, the PS ball arrays of the uniform solid matter of large area are prepared on a silicon substrate using liquid level assembling；Then PS will be covered with
The silicon substrate of array carries out oxygen plasma processing, power 30W, time 1h so that PS bulb diameters are less than 500nm after processing.
After oxygen plasma processing is carried out to PS ball arrays, sample is put into ion implantation apparatus and performed at ion irradiation
Reason, Implantation Energy 20keV, dosage are 1 × 1017ions/cm2。
Then, nanometer pinpoint template is coated into PDMS, 4000 revs/min of rotating speed, 30 seconds time；PDMS needs mixing cured
Agent stirs (PDMS:Curing agent=10:1), and using centrifuge there is no bubble into solution.
Then, sample is put into baking oven baking, temperature is 70 DEG C, and the time is 1 hour., will after treating that PDSM is fully cured
PDMS is stripped down.
Next, by spin-coating method on PET one layer of NOA61 uv-curable glue of spin coating.Will after spin coating uv-curable glue
The PDMS templates stripped down, which are pressed on PET, carries out ultraviolet light irradiation 30 minutes, then peels off PDMS templates.
As shown in fig. 6, PS balls are nearly all etched away, nanometer pinpoint array can not be obtained, illustrates that irradiation dose is excessive, no
Beneficial to the preparation of nanometer pinpoint array.
Above example is only the illustration done to technical solution of the present invention.It is involved in the present invention transparent soft
Property substrate on prepare the method for nanometer pinpoint array and be not merely defined in content described in the embodiment above, but with
Claim limited range is defined.What those skilled in the art of the invention were done on the basis of the embodiment any repaiies
Change or supplement or equivalence replacement, all in the claimed scope of the claim of the present invention.
Claims (8)
- A kind of 1. method that nanometer pinpoint array is prepared on transparent flexible substrate, it is characterised in that comprise the following steps：Step 1. prepares PS ball array templates by liquid level self assembly；Step 2. constructs nanometer pinpoint array template using the irradiation of oxygen plasma etch coupled ion beam on substrate；Step 3. spin coating PDMS on substrate of the surface with nanometer pinpoint array template, then peel off and obtain PDMS templates；Step 4. one layer of ultra-violet curing photo etching of spin coating on transparent flexible substrate, PDMS templates are pressed on transparent flexible substrate, After being solidified using uv light irradiation, take PDMS templates off, obtain nanometer pinpoint array.
- 2. the method according to claim 1 that nanometer pinpoint array is prepared on transparent flexible substrate, it is characterised in that：Wherein, in step 2, the ion beam used is nitrogen ion beam, irradiation energy 20keV, irradiation dose be more than or equal to 3 × 1016ions/cm2, and less than 1 × 1017ions/cm2。
- 3. the method according to claim 1 that nanometer pinpoint array is prepared on transparent flexible substrate, it is characterised in that：Wherein, in step 3, the substrate that spin coating has PDMS is put into baking oven and is heated to 50~70 DEG C, and it is small to be incubated 1~2 When, strip operation is then carried out again.
- 4. the method according to claim 1 that nanometer pinpoint array is prepared on transparent flexible substrate, it is characterised in that：Wherein, in step 3, be mixed with curing agent in PDMS, both be mixed evenly before spin coating, and centrifuged with Eliminate bubble.
- 5. the method according to claim 1 that nanometer pinpoint array is prepared on transparent flexible substrate, it is characterised in that：Wherein, in step 4, transparent flexible substrate is PET film substrate.
- 6. the method according to claim 1 that nanometer pinpoint array is prepared on transparent flexible substrate, it is characterised in that：Wherein, in step 4, ultra-violet curing photo etching is NOA61.
- 7. the method according to claim 1 that nanometer pinpoint array is prepared on transparent flexible substrate, it is characterised in that：Wherein, in step 4, the parameter of spin coating ultra-violet curing photo etching is 3000~5000 revs/min, 30~60 seconds.
- 8. the method according to claim 1 that nanometer pinpoint array is prepared on transparent flexible substrate, it is characterised in that：Wherein, in step 4, ultraviolet irradiation hardening time is 30 minutes.
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Cited By (1)
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