CN104829854B - A kind of preparation method and its product and purposes of the Block Copolymer Thin Film of vertical orientated self assembly - Google Patents
A kind of preparation method and its product and purposes of the Block Copolymer Thin Film of vertical orientated self assembly Download PDFInfo
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Abstract
The invention discloses the control method that a kind of block polymer forms vertical orientated package assembly.A variety of polystyrene b polymethacrylates (PS b PMA) of the block polymer comprising different molecular weight and block ratio.The vertical orientated control method is uniformly to spread in PS b PMA films in the surface weak inductive by electron beam irradiation or the substrate of insulation, is made by heating anneal.The accuracy controlling of small area pattern that control method vertical orientated PS b PMA proposed by the present invention has the pattern that novelty is strong, operating process simple, can form personalization, layer is regulated and controled without interface and can realize macroscopical large area morphogenesis and microcosmic.
Description
Technical field
The invention belongs to Macromolecular self-assembly field, in particular, it is related to a kind of block of vertical orientated self assembly and is total to
The preparation method and its product and purposes of homopolymer film.
Background technology
Nano-patterning technology based on block polymer film, due to block polymer can assemble to be formed size it is small and
Controllable (5-100nm), structure is adjustable (spherical, column, stratiform etc.), be easily achieved the series of advantages such as large area assembling, turns into
A kind of effective ways of patterned surface.This nano-patterning technology based on block polymer film is in microelectronics
The fields such as device, magnetic energy-storage device, multi-hole filtering film illustrate potential application prospect.
In order to realize the application of the nanolithographic based on block polymer, the pattern orientation of its film need to be controlled,
It is desirably to obtain vertical orientated stratiform or column structure.Researcher has had been developed that regulation and control interface or can utilize electric field, solvent
Control block polymer thin film alignment.Wherein use and construct electrode in film upper and lower interface, applying constant electric field can be with
The direction that is oriented along electric field line of induction block polymer is arranged, and then is formd and taken with substrate presentation vertical relation
To the formation (Science, 2000,290,2126-2129) of structure.But such a method electrode structure for constructing electric field is complicated, and
Needing block polymer film has the thickness of micron level in order to construct electrode and separation electrode, it is difficult to which the method is used
In the thin film system that thickness is Nano grade, and the lithographic technique based on block polymer is usually using the thin of Nano grade
Film.On the other hand, such a method for applying electric field is hardly formed the electric field of local or the electric field of small size and constructs out patterning
Package assembly.
Therefore it provides a kind of more convenient, general application electric field controls block polymer film process is for based on embedding
The patterning techniques of section polymer are significant, and also have theory value for block polymer assembling research.
The content of the invention
It is an object of the invention to overcome the defect of above-mentioned prior art common there is provided a kind of block of vertical orientated self assembly
The preparation method of homopolymer film, it is particularly a kind of that electrostatic is formed on weak inductive or dielectric base based on electron beam irradiation
, and then the method for controlling block copolymer pattern orientation.The method can obtain the controllable vertical orientated block of area and be total to
Homopolymer film.
It is another object of the present invention to provide a kind of the embedding of vertical orientated self assembly prepared by the above method
Section copolymer film, component containing the film and application thereof.
To achieve the above object, the present invention provides following technical scheme：
A kind of preparation method of the Block Copolymer Thin Film of vertical orientated self assembly, namely a kind of block copolymer form vertical
The control method of straight orientation self-assembled structures, it comprises the following steps：
(1) substrate of a surface weak inductive or insulation is provided；
(2) the above-mentioned substrate of electron beam irradiation is used；
(3) film of the block copolymer is sprawled in the above-mentioned substrate surface after electron beam irradiation；
(4) film of self assembly step (3), obtains the Block Copolymer Thin Film of the vertical orientated self assembly of the present invention；
Wherein, the block copolymer is that the block copolymer of polystyrene and polymethacrylates (is designated as PS-b-
PMA)。
According to the present invention, the areal extent of the Block Copolymer Thin Film is adjustable to Centimeter Level for nanoscale.Self assembly is walked
Suddenly the area for the film of the present invention that (4) one-shot forming is obtained can be nanoscale, or micron order, or be Centimeter Level,
Institute can realize that area is adjustable with the inventive method.
According to the present invention, the electron beam irradiation of the step (2) includes：By surface weak inductive or the substrate of insulation through electricity
Beamlet radiates doses.
Wherein, the surface weak inductive or the substrate of insulation include surface and contain the silicon base of spontaneous oxidation layer, surface
Silicon base, insulator simple glass containing artificial silica oxide layer, nitridation silicon base, insulation film polyimides or poly-
PVF is birdsed of the same feather flock together polymer substrates.
Wherein, the electron beam irradiation is that substrate is radiated using the equipment containing electron gun.
Wherein, the dosage of the electron beam irradiation refers to electron beam current × radiated time ÷ swept areas.
Wherein, the electron beam irradiation doses refer to be completely formed vertical orientated block in electron beam irradiation region
Dosage needed for copolymer film, it is preferable that the dosage of electron beam is not less than 20mC/cm2, electron beam current density is not more than
1000A/cm2, electron accelerating voltage is not less than 2kV.
Wherein, the swept area is 100nm2-1cm2。
According to the present invention, the block copolymer of the step (3) sprawl including：The block copolymer is dissolved in solvent
Middle acquisition solution, afterwards uniformly spreads in the solution in the substrate by electron beam irradiation.
Wherein, in the block copolymer molecular weight of polystyrene between 2 × 104~1 × 105Between, preferably 3 × 104
~8 × 104；The molecular weight of polymethacrylates is between 0.5 × 104~1 × 105Between, preferably 1 × 104~7 × 104。
Wherein, the self assembly of the block copolymer of step (4) is vertically oriented, with column structure or stratiform knot
Structure.For the PS-b-PMA of layer structure, the block ratio of polystyrene and polymethacrylates between 0.8~1.2,
It is preferably between 0.9~1.1；For the PS-b-PMA of column structure, the block ratio of polystyrene and polymethacrylates
Example is preferably between 1.8~2.2 between 1.5~2.5.
Wherein, the polymethacrylates is preferably polymethylacrylic acid C1-C4 Arrcostabs, such as polymethylacrylic acid
The positive fourth of methyl esters, polyethyl methacrylate, poly-n-propyl methacrylate, polyisopropyl methacrylate, polymethylacrylic acid
Ester, polyisobutyl methacrylate or polymethyl tert-butyl acrylate etc., more preferably polymethyl methacrylate (PMMA).
Wherein, the concentration of the block copolymer solution is 2-20mg/ml.
Wherein, the method uniformly sprawled includes drop coating, spin coating, spraying etc..
According to the present invention, the polymer self assembles of the step (4) include：The PS-b-PMA films that will be spread in substrate
Heating anneal, is cooled to the Block Copolymer Thin Film that the self assembly is obtained after room temperature.
Wherein, the heating anneal refers to anneal Block Copolymer Thin Film in inert atmosphere or heated under vacuum,
The temperature of heating anneal is 170-250 DEG C, and the time is 2-30h.
The present invention also provides following technical scheme：
A kind of Block Copolymer Thin Film of the vertical orientated self assembly prepared by the above method, the block copolymer
It is the block copolymer (being designated as PS-b-PMA) of polystyrene and polymethacrylates, the self assembly of the block copolymer is
Vertical orientated, with column structure or layer structure, the area of the structure with self assembly can be 100nm2~
1cm2, the thickness of the film is 30nm~200nm.
In the present invention, vertical relation is presented with substrate in the vertical orientated structure for referring to PS-b-PMA thin-film self-assemblings
Pattern.
According to the present invention, for layer structure, finger print is presented in its surface texture；For column structure, its surface
The arrangement of six sub-symmetry lattice-likes is presented in structure.
According to the present invention, the molecular weight of polystyrene is between 2 × 10 in block copolymer4~1 × 105Between, preferably 3 ×
104~8 × 104；The molecular weight of polymethacrylates is between 0.5 × 104~1 × 105Between, preferably 1 × 104~7 × 104。
According to the present invention, for the PS-b-PMA of layer structure, the block ratio of polystyrene and polymethacrylates
Between 0.8~1.2, it is preferably between 0.9~1.1；For the PS-b-PMA of column structure, polystyrene and poly- methyl
The block ratio of acrylate is preferably between 1.8~2.2 between 1.5~2.5.
According to the present invention, the polymethacrylates is preferably polymethylacrylic acid C1-C4 Arrcostabs, such as poly- methyl
Methyl acrylate, polyethyl methacrylate, poly-n-propyl methacrylate, polyisopropyl methacrylate, polymethyl
Sour N-butyl, polyisobutyl methacrylate or polymethyl tert-butyl acrylate etc., more preferably polymethyl methacrylate.
A kind of component, it includes the substrate of a surface weak inductive or insulation, and is formed at above-mentioned in the substrate
The Block Copolymer Thin Film of vertical orientated self assembly；The film is thin by the block copolymer of above-mentioned vertical orientated self assembly
The preparation method of film is formed in the substrate.
According to the present invention, the substrate include surface contain spontaneous oxidation layer silicon base, surface contain artificial titanium dioxide
Silicon base, insulator simple glass, nitridation silicon base, insulation film polyimides or the polyvinyl-fluoride polymer of silicon oxide layer
Substrate.
The present invention also provides the purposes of said modules, and specifically, the component is in microelectronic component, photoelectric device, magnetic
There is potential purposes in the fields such as memory device, porous UF membrane.
According to the present invention, the Block Copolymer Thin Film for the vertical orientated self assembly that the component includes can be as nanometer
Material pattern, the nano material for forming pattern structure.
The beneficial effects of the invention are as follows：
The present invention provides a kind of preparation method of the Block Copolymer Thin Film of vertical orientated self assembly, namely one kind vertically takes
To Block Copolymer Thin Film self-assembled structures control method, methods described has that novelty is strong, operating process simple, can be with
Small area pattern form personalized pattern, layer is regulated and controled without interface and can realize macroscopical large area morphogenesis and microcosmic
Accuracy controlling (different demands that large area and small area can be achieved).
The thickness of the Block Copolymer Thin Film for the vertical orientated self assembly that the above method of the present invention is prepared is nanometer
Level, and the structure of its self assembly can be adjusted between micron to nano grade, that is to say, that it is controllable, personalized with size
The various vertical orientated pattered region of microscopic appearance；Component containing the film is in microelectronic component, photoelectric device, magnetic storage
There is potential purposes in the fields such as memory device, porous UF membrane.
Brief description of the drawings
Fig. 1 is the route schematic diagram of the preparation method of the present invention.
Fig. 2 is the electron scanning micrograph of the PS-b-PMMA film surface appearances of the column structure of embodiment 1：a)
For low power number photo, b) it is high magnification numbe photo.
Fig. 3 is the electron scanning micrograph of the PS-b-PMMA film surface appearances of the column structure of comparative example 1.1.
Fig. 4 is the electron scanning micrograph of the PS-b-PMMA film surface appearances of the layer structure of embodiment 2.
Fig. 5 is the electron scanning micrograph of the PS-b-PMMA film surface appearances of the column structure of embodiment 3.
Fig. 6 is the electron scanning micrograph of the PS-b-PMMA film surface appearances of the column structure of embodiment 4：a)
For low power number photo, b) it is high magnification numbe photo.
Fig. 7 is the electron scanning micrograph of the PS-b-PMMA film surface appearances of the column structure of embodiment 5：a)
For low power number photo, b) it is high magnification numbe photo.
Embodiment
Below in conjunction with drawings and examples, the present invention is described in further detail.But skilled in the art realises that,
Protection scope of the present invention is not limited only to following examples.According to present disclosure, those skilled in the art will recognize that
To in the case where not departing from the technical characteristic and scope given by technical solution of the present invention, embodiment described above is made perhaps
Change and modifications belongs to protection scope of the present invention more.
Experimental method described in following embodiments, is conventional method unless otherwise specified；The reagent and material,
Commercially obtain.
Used in following each embodiments to PS-b-PMMA series block copolymers be purchased from Canadian Polymer
Source companies.
Embodiment 1
Fig. 1 is shown as a kind of route signal of control method of the self-assembled structures of vertical orientated PS-b-PMMA films
Figure.
(1) electron beam irradiation
Electron beam is by 5kV of accelerating potential, electron beam current is 16.7pA, radiated time is 6min (360s), radiating surface
Product is 11.32 μm2(i.e. dose of radiation is 53mC/cm2) radiation containing spontaneous oxidation layer silicon base surface.
(2) block copolymer is sprawled
Concentration is spin-coated on electron beam irradiation for 9mg/ml PS-b-PMMA (46k-b-21k) solution with 2000rpm, 40s
In silicon base afterwards.
(3) polymer self assembles
Substrate containing PS-b-PMMA films is placed in Ar atmosphere in tube furnace and encloses lower 250 DEG C of annealing 2h, room is cooled to
Temperature, completes self assembly.
Scanning electron microscopy is used after the film after annealing finally is etched into (20sccm, 50W, 5min) through argon plasma
Its surface topography of sem observation.Fig. 2 is the surface topography map of the PS-b-PMMA films for the column structure that embodiment 1 is obtained.Formed
Six times regular cavernous structures prove which form vertical orientated column structure.
Comparative example 1.1
Other conditions are same as Example 1, the difference is that only (one) electron beam irradiation, radiated time be 2min (i.e.
Dose of radiation is 17.7mC/cm2).Fig. 3 is the surface topography of the PS-b-PMMA films for the column structure that comparative example 1.1 is obtained
Figure.The central area does not form six cavernous structures.This comparative example illustrates that doses of electron beam radiation is that control film is formed
Vertical orientated key factor.
Embodiment 2
(1) electron beam irradiation
Electron beam is by 5kV of accelerating potential, electron beam current is 16.7pA, radiated time is 3min, swept area is
11.32μm2(i.e. dose of radiation is 26.5mC/cm2) radiation containing artificial oxide layer silicon base surface.
(2) block copolymer is sprawled
By concentration for 11mg/ml PS-b-PMMA (53k-b-54k) solution with 2000rpm, 40s is spin-coated on electron beam spoke
In silicon base after penetrating.
(3) polymer self assembles
Substrate containing PS-b-PMMA films is placed in Ar atmosphere in tube furnace and encloses lower 250 DEG C of annealing 2h, room is cooled to
Temperature, completes self assembly.
Its surface topography is observed with SEM after handling as described in Example 1.Fig. 4 is that embodiment 2 is obtained
Layer structure PS-b-PMMA films surface topography map.The finger print structure of formation prove form it is vertical orientated
Layer structure.
Embodiment 3
(1) electron beam irradiation
Electron beam is by 5kV of accelerating potential, electron beam current is 16.7pA, the dose of radiation of electron beam is 50mC/cm2、
Radiation areas radiate the surface of the silicon base containing spontaneous oxidation layer for a diameter of 100nm border circular areas.
(2) block copolymer is sprawled
Concentration is spin-coated on electron beam irradiation for 9mg/ml PS-b-PMMA (46k-b-21k) solution with 2000rpm, 40s
In silicon base afterwards.
(3) polymer self assembles
Substrate containing PS-b-PMMA films is placed in Ar atmosphere in tube furnace and encloses lower 250 DEG C of annealing 2h, room is cooled to
Temperature, completes self assembly.
Its surface topography is observed with SEM after handling as described in Example 1.Fig. 5 is that embodiment 3 is obtained
Column structure PS-b-PMMA films surface topography map.The regular cavernous structure of formation is then proved to form and vertically taken
To column structure.Isolated or a pair of holes of embodiment formation show that the swept area and radiation agent of electron beam can be controlled
Amount, obtains vertical orientated PS-b-PMMA films in the surface area of the limit.
Embodiment 4
(1) electron beam irradiation
Electron beam is by 15kV of accelerating potential, electron beam current is 100nA, radiated time is 60min, swept area is
6.75mm2(i.e. dose of radiation is 53.3mC/cm2) radiation containing spontaneous oxidation layer silicon base surface.
(2) block copolymer is sprawled
By PS-b-PMMA (46k-b-21k) the solution drop coating in silicon base after electron beam irradiation of concentration for 9mg/ml.
(3) polymer self assembles
Substrate containing PS-b-PMMA films is placed in Ar atmosphere in tube furnace and encloses lower 250 DEG C of annealing 2h, room is cooled to
Temperature, completes self assembly.
Its surface topography is observed with SEM after handling as described in Example 1.Fig. 6 is that embodiment 4 is obtained
Column structure PS-b-PMMA films surface topography map.The regular six time cavernous structure formed then proves shape
Into vertical orientated column structure.And 6a is shown as the film of the homogeneous contrast of large area, shows by controlling electron beam
Swept area and radiated time, can obtain the vertical orientated PS-b-PMMA films of large area region.
Embodiment 5
(1) electron beam irradiation
Electron beam is by 5kV of accelerating potential, electron beam current is 21pA, dose of radiation is 50mC/cm2Radiation is containing spontaneous
The surface of the silicon base of oxide layer, electron beam irradiation mode be according to program setting route selection substrate regional area
Radiated.Radiation areas are letter NANO patterns.
(2) block copolymer is sprawled
By PS-b-PMMA (46k-b-21k) the solution drop coating in silicon base after electron beam irradiation of concentration for 9mg/ml.
(3) polymer self assembles
Substrate containing PS-b-PMMA films is placed in Ar atmosphere in tube furnace and encloses lower 250 DEG C of annealing 2h, room is cooled to
Temperature, completes self assembly.
Fig. 7 is the surface topography map of the PS-b-PMMA films for the column structure that embodiment 5 is obtained.In the alphabetical region
Form vertical orientated pore space structure.The example shows that the method for such a electron beam regulation and control block copolymer orientation (self assembly) can
To form the vertical orientated pattered region that controllable, the personalized microscopic appearance of size is various.
The description of exemplary type is done to the present invention above, it should be appreciated that in the case where not departing from the core of the present invention,
Any simple deformation, modification or other skilled in the art can not spend the equivalent substitute of creative work to each fall within this
The protection domain of invention.
Claims (23)
1. a kind of preparation method of the Block Copolymer Thin Film of vertical orientated self assembly, namely a kind of block copolymer are formed vertically
The control method of self-assembled structures is orientated, it comprises the following steps：
(1) substrate of a surface weak inductive or insulation is provided；
(2) the above-mentioned substrate of electron beam irradiation is used；
(3) film of the block copolymer is sprawled in the above-mentioned substrate surface after electron beam irradiation；
(4) film of self assembly step (3), obtains the Block Copolymer Thin Film of described vertical orientated self assembly；
Wherein, the block copolymer is the block copolymer of polystyrene and polymethacrylates, is designated as PS-b-PMA.
2. preparation method according to claim 1, it is characterised in that the areal extent of the Block Copolymer Thin Film is to receive
Meter level is adjustable to Centimeter Level.
3. preparation method according to claim 1 or 2, it is characterised in that the electron beam irradiation of the step (2) includes：
By surface weak inductive or the substrate of insulation through electron beam irradiation doses；
The dosage of the electron beam irradiation refers to electron beam current × radiated time ÷ swept areas；
The electron beam irradiation doses refer to be completely formed vertical orientated block copolymer in electron beam irradiation region thin
Dosage needed for film.
4. preparation method according to claim 3, it is characterised in that the surface weak inductive or the substrate of insulation include
Surface contain spontaneous oxidation layer silicon base, surface contain artificial silica oxide layer silicon base, insulator simple glass,
Nitrogenize silicon base, insulation film polyimides or polyvinyl-fluoride polymeric substrates.
5. preparation method according to claim 3, it is characterised in that the electron beam irradiation is using containing electron gun
Equipment is radiated to substrate.
6. preparation method according to claim 3, it is characterised in that the dosage of electron beam is not less than 20mC/cm2, electron beam
Current density is not more than 1000A/cm2, electron accelerating voltage is not less than 2kV；The swept area is 100nm2-1cm2。
7. preparation method according to claim 1, it is characterised in that the block copolymer of the step (3) sprawl including：
The block copolymer is dissolved in solvent and obtains solution, afterwards uniformly spreads in the solution by electron beam irradiation
In substrate.
8. preparation method according to claim 1, it is characterised in that the molecular weight of polystyrene in the block copolymer
Between 2 × 104~1 × 105Between；The molecular weight of polymethacrylates is between 0.5 × 104~1 × 105Between.
9. preparation method according to claim 8, it is characterised in that the molecular weight of polystyrene in the block copolymer
Between 3 × 104~8 × 104Between；The molecular weight of polymethacrylates is between 1 × 104~7 × 104Between.
10. preparation method according to claim 1, it is characterised in that the self assembly of the block copolymer of step (4)
It is vertically oriented, with column structure or layer structure；
For the PS-b-PMA of layer structure, the block ratio of polystyrene and polymethacrylates between 0.8~1.2 it
Between；
For the PS-b-PMA of column structure, the block ratio of polystyrene and polymethacrylates between 1.5~2.5 it
Between.
11. preparation method according to claim 10, it is characterised in that for the PS-b-PMA of layer structure, polyphenyl second
The block ratio of alkene and polymethacrylates is between 0.9~1.1；
For the PS-b-PMA of column structure, the block ratio of polystyrene and polymethacrylates between 1.8~2.2 it
Between.
12. preparation method according to claim 1, it is characterised in that the polymethacrylates is polymethyl
Sour C1-C4 Arrcostabs.
13. preparation method according to claim 12, it is characterised in that the polymethacrylates is polymethyl
Sour methyl esters, polyethyl methacrylate, poly-n-propyl methacrylate, polyisopropyl methacrylate, polymethylacrylic acid are just
Butyl ester, polyisobutyl methacrylate or polymethyl tert-butyl acrylate.
14. preparation method according to claim 7, it is characterised in that the concentration of the block copolymer solution is 2-
20mg/ml。
15. preparation method according to claim 7, it is characterised in that the method uniformly sprawled includes drop coating, spin coating
Or spraying.
16. preparation method according to claim 1, it is characterised in that the polymer self assembles of the step (4) include：
By the PS-b-PMA film heatings spread in substrate annealing, be cooled to obtained after room temperature the self assembly block copolymer it is thin
Film.
17. preparation method according to claim 16, it is characterised in that the heating anneal refers to block copolymer is thin
Film is annealed in inert atmosphere or heated under vacuum, and the temperature of heating anneal is 170-250 DEG C, and the time is 2-30h.
18. a kind of block copolymer for the vertical orientated self assembly that method as described in claim any one of 1-17 is prepared
Film, the block copolymer is the block copolymer of polystyrene and polymethacrylates, is designated as PS-b-PMA, described embedding
What the self assembly of section copolymer was vertically oriented, with column structure or layer structure, the face of the structure with self assembly
Product is 100nm2~1cm2, the thickness of the film is 30nm~200nm；
The pattern of vertical relation is presented with substrate for the vertical orientated structure for referring to PS-b-PMA thin-film self-assemblings.
19. Block Copolymer Thin Film according to claim 18, it is characterised in that for layer structure, its surface knot
Finger print is presented in structure；For column structure, the arrangement of six sub-symmetry lattice-likes is presented in its surface texture.
20. a kind of component, it includes the substrate of a surface weak inductive or insulation, and the claim being formed in the substrate
The Block Copolymer Thin Film of vertical orientated self assembly described in 18 or 19；The film passes through described in claim any one of 1-17
The preparation method of Block Copolymer Thin Film of vertical orientated self assembly be formed in the substrate.
21. component according to claim 20, it is characterised in that the substrate includes the silicon that spontaneous oxidation layer is contained on surface
Substrate, surface contain the silicon base of artificial silica oxide layer, insulator simple glass, nitridation silicon base, insulation film and gathered
Acid imide or polyvinyl-fluoride polymeric substrates.
22. the purposes of component described in claim 20 or 21, it is characterised in that the component is used for following fields：Microelectronics device
Part, photoelectric device, magnetic memory device or porous UF membrane.
23. purposes according to claim 22, it is characterised in that the vertical orientated self assembly that the component includes it is embedding
Section copolymer film is as nano material template, the nano material for forming pattern structure.
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| CN103839785A (en) * | 2012-11-27 | 2014-06-04 | 国际商业机器公司 | Method for forming photo composition |
Non-Patent Citations (3)
| Title |
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| Orientation change of diblock copolymer thin films by the addition of amphiphilic surfactants: effect of film thickness and surfactant concentration;Jeong Gon Son, etal.;《Macromolecules》;20111205;第45卷(第1期);第150-158页 * |
| Ultrahigh-Density Nanowire Arrays Grown in;Thurn-Albrecht T，etal;《Science》;20001215;第290卷(第5499期);第2126-2129页 * |
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