CN107522163B - A kind of high guarantor's type transfer method of PDMS structure - Google Patents
A kind of high guarantor's type transfer method of PDMS structure Download PDFInfo
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- CN107522163B CN107522163B CN201710480011.8A CN201710480011A CN107522163B CN 107522163 B CN107522163 B CN 107522163B CN 201710480011 A CN201710480011 A CN 201710480011A CN 107522163 B CN107522163 B CN 107522163B
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- B81B7/00—Microstructural systems; Auxiliary parts of microstructural devices or systems
- B81B7/02—Microstructural systems; Auxiliary parts of microstructural devices or systems containing distinct electrical or optical devices of particular relevance for their function, e.g. microelectro-mechanical systems [MEMS]
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Abstract
The invention discloses a kind of high guarantor's type transfer methods of PDMS structure, can be used for the preparation of the flexible multi-layered micro-nano structure of PDMS.This method prepares the silicon template 2 of PDMS structure to be transferred first；Make PDMS transfer layer 5；The PDMS solution that the quasi- amount of drop is slowly tried along silicon template center, scatters from face center toward surrounding to it, slowly flows into each structural cavities, it is desirable that PDMS solution does not spill over silicon wafer template surface with exterior domain；Using PDMS transfer layer 5, it is placed in the one side that silicon template 2 has PDMS structure, uniformly applies pressure, is put into after solidifying in insulating box and take out, then remove silicon template 2, the PDMS structure in such silicon template 2 in each structural cavities is transferred on PDMS transfer layer 5 with regard to guarantor's type.Present invention process process is relatively easy, provides important leverage for preparation multilayer micro-nano structure technique, also the application for shifting process in other micro-nano structures preparation process provides new solution.
Description
Fields
The invention belongs to integrated circuit and micro-nano electronic mechanical system production field more particularly to a kind of height of PDMS structure
Guarantor's type transfer method, can be used for the preparation of the flexible multi-layered micro-nano structure of PDMS.
Background technique
The not contour micro-nano structure of multilayer in bionics, in optics, Surface Science, before medicine and other fields extensive application
Scape.Multilayer micro-nano structure is super-hydrophobic anti-freeze, and extensive research and application have been carried out in the fields such as heat transmitting.Poly- diformazan
Radical siloxane (PDMS) is a kind of common polymer material in laboratory, has preferable hydrophobicity, flexible and elasticity, thermostabilization
Property, antiacid alkali and organic solvent, advantages of environment protection, laboratory carries out the preparation of micro-nano structure through commonly using this material.In order to
The not contour micro-nano structure of multilayer is prepared, the not contour structure of multilayer is divided into each only by the present method using successively transfer assembling
Then each structure sheaf is transferred on PDMS transfer layer by the method that structure shifts, then passes through alignment again by vertical single layer
Structure on each PDMS transfer layer is successively transferred to PDMS structured base layer up by sequence from low to high by the mode of bonding,
Complete the preparation of the not contour micro-nano structure of multilayer.The not contour micro-nano structure of multilayer is prepared in the method using successively transfer assembling
When, guarantee that each PDMS high guarantor's type transfer preparation layered is an important problem.In existing PDMS structure preparation, it is
PDMS is spun on stay in place form, peels from a template to obtain desired PDMS structure after PDMS solidification, it at all can not shape
It is shifted at guarantor's type of required PDMS structure.
When transfer organization, usually due to silicon mould and apply between load layer there are the problems in stress collection, so as to cause
When PDMS transfer layer is bonded by extraneous load with silicon wafer mold, because PDMS transfer layer itself is flexible material, due to answering
The problems in power collection, causes PDMS transfer layer micro-strain occur, and this micro-strain prepares micron-sized structure for transfer
It usually influences very big, in turn results in be transferred out structure sheaf appearances, the problems such as torsional deformation, pattern are distorted, be unable to complete
High guarantor's type of structure sheaf shifts, and shifts fragrant method still without high guarantor's type about micro-nano structure at present, turns to solve micro-nano structure
Process difficulties during shifting propose a kind of high guarantor's type transfer method of completely new PDMS structure.
Summary of the invention
The purpose of the present invention is: PDMS structure is transferred to up from silicon template by PDMS transfer layer using the method for transfer,
The technological problems such as distortion, torsional deformation of size and shape of structure in PDMS flexible structure shifting process can be faced.The present invention
It solves the problems, such as to shift in existing technology without PDMS structure height guarantor's type.
In view of the above-mentioned problems, the technical scheme is that a kind of high guarantor's type transfer method of PDMS structure, including it is as follows
Step:
Step 1: the silicon template 2 of PDMS structure to be transferred is prepared；Specifically include following sub-step:
Sub-step one: silicon wafer mask plate is prepared；
Sub-step two: carrying out photoetching and dry etching to monocrystalline silicon 1 with mask plate prepared by sub-step one, needed for obtaining to
Shift the silicon template 2 of PDMS structure；
Step 2: production PDMS transfer layer 5；Specifically include following sub-step:
Sub-step one: preparation PDMS blanket layer 3；
As the more excellent scheme in the sub-step, which prepares mold I by production PDMS transfer layer, then will
After proportioned PDMS and curing agent are vacuum-treated, pour into PDMS transfer layer mold I and realized after solidification；The system
Make the detailed process of PDMS transfer layer preparation mold I are as follows: take two pieces of clean 6, four pieces of organic glass pads of quartz glass plate
7, four binder clips of block 8, one solid flexible rubber circles, are placed on one of quartz glass plate 6 for solid flexible rubber circle 7
On surround an open cylindrical cavity, organic glass cushion block 8 is placed on to four positions of rubber ring 7, then by other one block of quartz
Glass plate 6 is covered on the direction of the nethermost quartz glass plate 6 of face and forms PDMS transfer layer above and prepare mold cavity I, so
Uniformly step up to fix along four direction with binder clip afterwards.
Sub-step two: PDMS blanket layer 3 prepared by sub-step one and a culture dish are put into vitreous evacuated container, are carried out
It vacuumizes, then by intake valve toward injection this inert gas of nitrogen in cabinet until inside and outside air pressure balance；Case is opened rapidly
Body simultaneously drips silicon fluoride solution into culture dish, then closes cabinet rapidly and carries out vacuum pumping immediately, when standing one section
Between, it is taken out after 3 surface of PDMS blanket layer deposited one layer of silicon fluoride；Nitrogen during this is that prevent will as protection gas
The silicon fluoride oxidation deactivation of instillation；
Sub-step three: by sub-step bifluoride treated PDMS blanket layer 3 is put into keep the temperature a period of time in insulating box after
It takes out；The process is to make silicon fluoride layer 4 on its surface to complete the molecule of silicon fluoride layer 4 and 3 surface of PDMS blanket layer and assemble
It is above more stable to retain.
So far, the production of PDMS transfer layer 5 is completed.
Step 3: along the PDMS solution of the center of silicon template 2 of the step 1 slowly quasi- amount of examination drop, to it from face center toward four
Week scatters, and slowly flows into each structural cavities, it is desirable that PDMS solution does not spill over silicon wafer template surface with exterior domain；
Step 4: the PDMS transfer layer 5 made using step 2, being placed in silicon template 2 in step 3 has the one of PDMS structure
Face uniformly applies pressure, is put into after solidifying in insulating box and takes out, then removes silicon template 2, each structure in such silicon template 2
PDMS structure in cavity is transferred on PDMS transfer layer 5 with regard to guarantor's type；
In order to preferably uniformly apply pressure to PDMS transfer layer 5 in this process, the present invention is as a kind of more excellent side
Case loads cavity using high precision silicon template come what is realized, and detailed process includes following sub-step:
Sub-step one: one piece of clean quartz glass plate 6 is taken, one piece and used silicon wafer mould are fixed in region in its center
Has the silicon template 2 of comparable size.
Sub-step two: one piece of clean solid flexible rubber of 6, four pieces of quartz glass plate organic glass cushion block 8, one is separately taken
7, four binder clips are enclosed, silicon template 2 is fixed on 6 centre of surface position of quartz glass plate, solid flexible rubber circle 7 is placed on
On the quartz glass plate 6 of sub-step one and an open cylindrical cavity is surrounded, organic glass cushion block 8 is placed on solid flexible rubber circle
Then other one piece of quartz glass plate 6 is covered on by 7 four positions with the direction of the nethermost quartz glass plate 6 of face
Face composition high precision silicon template loading mold 9 prepares chamber II, then uniformly steps up to fix along four direction with binder clip.
Sub-step three: it prepares to pour into chamber II toward the high precision silicon template loading mold 9 that sub-step two obtains and matches
PDMS solution 10, be then placed in solidification in insulating box.PDMS high precision silicon template loading mold 9II is integrally taken after being cured
Out.Silicon template 2 is put into the high precision silicon template loading mold 9, so that 2 surface of silicon template and high precision silicon template loading mold
9 upper surfaces keep concordant.
It goes to load silicon template 2 using the high precision silicon template loading mold 9, acts on PDMS turns when applying uniform load 11
When moving layer 5, PDMS transfer layer 5 and silicon template 2 there would not be the problems in contact edge stress collection, and silicon template 2 and PDMS turn
Shifting layer 5 acts on lower stress in uniform load 11 can be more balanced.Optimize high guarantor's type process transfer method.Beneficial effects of the present invention
It is: solves the defective workmanships such as structural distortion, the deformation when preparing multilayer micro-nano structure with the method for transfer assembling.Micro-structure turns
The key for moving technique is the problem of stress concentration being easy in silicon template 2 and the contact line of PDMS transfer layer 5 when applying load,
It because PDMS transfer layer 5 is flexible material in itself, thus is particularly easy to cause to deform, so as to cause PDMS transfer layer is eventually transferred into
There is the problems such as deformation, distortion and high distortion in structure on 5, makes 500 μm of height in turn by the method for making PDMS plate
Precision silicon template loading mold 9, and then the standard wafer silicon wafer mold with a thickness of 500 μm can be embedded in high precision silicon template dress
It carries in mold 9, while being tested by serial experiment, in the case where PDMS transfer layer 5 can be transferred to by not influencing structure, improved
The proportion of PDMS and curing agent is ultimately determined to the ratio of 7:1 to improve the thickness of PDMS transfer layer 5, just reducing or
Eliminate the problem of stress concentration when structure sheaf is bonded with transfer layer.Technical process is relatively easy, to prepare multilayer micro-nano structure
Technique provides important leverage, and also the application for shifting process in other micro-nano structures preparation process provides new solution party
Case.
Detailed description of the invention
Fig. 1 is high guarantor's type shifting process flow chart proposed by the present invention.
Fig. 2 is that PDMS transfer layer preparation mold I and high precision silicon template loading mold prepare chamber II
Fig. 3 is that embodiment is finally completed big depth-of-field microscope observation chart when the transfer of high guarantor's type.
In figure: 1- monocrystalline silicon, 2- silicon template, 3-PDMS blanket layer, 4- silicon fluoride layer, 5-PDMS transfer layer, 6- quartz glass
Glass plate, the solid flexible rubber circle of 7-, 8- organic glass cushion block, 9- high precision silicon template loading mold, 10-PDMS solution, 11- are equal
Cloth load.
Specific implementation method
Embodiment 1:
This gives a kind of high guarantor's type transfer method of single layer structure, this layer of structure is circular cylindrical shape array structure
Layer.Designed structure size body diameter is 5 μm in this, and cylinder height is 8 μm, and the longitudinal pitch between cylinder is 10 μ
M, transverse pitch are 10 μm.High guarantor's type transfer method of the present embodiment single layer structure includes the following steps:
Step 1: the silicon template 2 of PDMS structure to be transferred is prepared；Specifically include following sub-step:
Sub-step one: silicon wafer mask plate is prepared；Rod array structure is designed by mask, array of structures size: circle
Column diameter is 5 μm, and cylinder height is 8 μm, and the longitudinal pitch between cylinder is 10 μm, and transverse pitch is 10 μm.
Sub-step two: carrying out photoetching to monocrystalline silicon with mask plate prepared by sub-step one, PDMS knot to be transferred needed for obtaining
The silicon template 2 of structure；Photoetching is etched using inductively coupled plasma precursor reactant, uses the design parameter of etching technics are as follows:
SF6, gas flow 180sccm/min, etch period 14s；C4F6, gas flow 85sccm/min, passivation time 7s；Etching/
The number of passivation cycle is 7-28 times；After etching, using O2 as working gas, photoresist is removed；
Step 2: production PDMS transfer layer；Specifically include following sub-step:
Sub-step one: preparation PDMS blanket layer 3；In the embodiment, first with the mass ratio proportion PDMS of 7:1 and solidification
Agent, wherein 21 grams of PDMS liquid, 3 grams of curing agent.The two is poured into respectively in culture dish and is stirred evenly, vacuum oven is put into
It is interior, to its vacuumize process, vacuum oven is closed when being evacuated to bubble-free in PDMS solution, it is taken out of vacuum oven
Out；Mold is prepared followed by production PDMS transfer layer: taking two pieces of clean quartz glass plates, four block size 2mm × 2mm
The organic glass cushion block of × 2mm, one in its natural state diameter be 3mm, length be 20mm solid flexible rubber circle, four
Solid flexible rubber circle is placed on one of quartz glass plate and surrounds an open cylindrical cavity, cushion block is placed by binder clip
In four positions of nylon rope, then other one piece of quartz glass plate is covered with the direction of the nethermost quartz glass plate of face
Mold is prepared in composition PDMS transfer layer above, then uniformly steps up to fix along four direction with binder clip；It will finally take out
The PDMS solution of good vacuum pours into made PDMS transfer layer preparation mold, is then wholy placed in insulating box
It is interior, with 60 DEG C of temperature, solidifies 8 hours, be drawn off after being cured, PDMS is taken out, is cured by mold of dismantling
The PDMS with a thickness of 2mm.
Sub-step two: PDMS blanket layer 3 prepared by sub-step one and a culture dish are put into vitreous evacuated container, into
Row vacuumizes until draught head is an atmospheric pressure, then by passing through intake valve toward injection this inert gas of nitrogen in cabinet
The silicon fluoride oxidation deactivation that will be instilled is prevented as protection gas, injection nitrogen gas is until inside and outside air pressure balance.Then rapidly
It opens cabinet and drips 2-3ml silicon fluoride solution into culture dish, then close cabinet rapidly and carry out vacuum pumping immediately,
Until inside and outside differential pressure is an atmospheric pressure.It is taken out after standing 3h.
Sub-step three: by sub-step bifluoride, treated that PDMS blanket layer 3 is put into insulating box with 60 degrees Celsius of temperature
Degree takes out after heat preservation a period of time；The process is to make fluorine to complete the molecule of silicon fluoride layer and 3 surface of PDMS blanket layer and assemble
Silylation layer is more stable on the surface thereof to retain.
So far, the production of PDMS transfer layer is completed.
Step 3: along the PDMS solution of the center of silicon template 2 of the silicon wafer one slowly quasi- amount of examination drop, to it from face center toward four
Week scatters, and slowly flows into each structural cavities, it is desirable that PDMS solution does not spill over 2 surface of silicon template with exterior domain；
Step 4: the PDMS transfer layer made using step 2, being placed in silicon template 2 in step 3 has the one of PDMS structure
Face uniformly applies pressure, is put into after solidifying in insulating box and takes out, then removes PDMS transfer layer, respectively tie in such silicon template 2
PDMS structure in structure cavity is transferred on PDMS transfer layer with regard to guarantor's type；
In order to preferably uniformly apply pressure to PDMS transfer layer in this process, using high-precision in the present embodiment
It spends silicon template and loads cavity come what is realized, detailed process includes following sub-step:
Sub-step one: matching PDMS liquid and curing agent with the mass ratio of 5:1, wherein 15 grams of PDMS liquid quality, Gu
Agent quality is 3 grams, pours into same glass container, carries out vacuumize process after mixing evenly through glass bar；
Sub-step two: production high precision silicon template loading mold prepares chamber: taking two pieces of clean quartz glass plates, four pieces
Size 2mm × 2mm × 2mm organic glass cushion block, one in its natural state diameter be 3mm, length be 20mm it is solid soft
Property rubber ring, four binder clips, solid flexible rubber circle is placed on one of quartz glass plate and surrounds an open circle
Cushion block is placed on four positions of solid flexible rubber circle by chamber, by the brilliant with a thickness of 500 μm of standard of one piece of 20mm × 20mm
Circle is fitted on the pieces of quartz glass plate with double-sided adhesive, then by other one piece of quartz glass plate with the nethermost quartzy glass of face
The direction of glass plate is covered on composition high precision silicon template loading mold above and prepares chamber, then equal along four direction with binder clip
It is even to step up to fix；
Sub-step three: after the completion of PDMS solidification, cavity of dismantling takes out prepared high precision silicon template loading mold.
High guarantor's type transfer process of silicon template micro-structure is divided into following sub-step in the present embodiment:
Sub-step one: liquid PDMS and curing agent are matched with the mass ratio of 10:1, carry out vacuumize process；
Sub-step two: tool: Bidirectional flat-nose pliers, having a size of two pieces of 50mm × 100mm × 10mm quartz glass, aluminium is taken out
Foil paper, double-sided adhesive.Aluminium-foil paper is cut, is entirely fitted on two pieces of quartz glass plates respectively by double-sided adhesive, by the inner system of step 5
Standby high precision silicon template loading mold is placed on wherein a piece of quartz glass plate, using the suction-operated of aluminium-foil paper and PDMS,
So that it is fitted in surface, the silicon template 2 for the structure to be shifted is put into high precision silicon template loading mold；
Sub-step three: it by PDMS solution obtained in sub-step one, takes a small amount of drop on 2 surface of silicon template, covers table to it
Face, then stand 10min wait for PDMS solution completely into silicon template 2, the PDMS transfer layer that step 2 is made, along stone
One side of English glass plate is gently twisted toward another side and is pressed, and guarantees to twist bubble-free in pressure and occurs, until being completely covered on the table of silicon template 2
Face.
Sub-step 4: placing Bidirectional flat-nose pliers vertically, and the PDMS transfer layer posted in sub-step three is connected with silicon template 2
It is placed on together with quartz glass plate on the lower clamping face of Bidirectional flat-nose pliers, then turns knob and decline upper clamping face, apply and carry
Lotus clamps.Entirety was put into insulating box, with temperature-curable 8 hours of 60 DEG C；
Sub-step five: after being cured, whole take out reversely rotates Bidirectional flat-nose pliers knob, clamping face is removed, by PDMS
Transfer layer integrally takes out together with the structure in silicon template 2, completes high guarantor's type transfer in the silicon template 2 of PDMS flexible structure.
Cavity is loaded using the high precision silicon template to go to load silicon template 2, when application load acts on PDMS transfer layer,
PDMS transfer layer and silicon template 2 there would not be the problems in contact edge stress collection, and silicon template 2 and PDMS transfer layer are in load
Acting on lower stress can be more balanced.Optimize high guarantor's type process transfer method.The big depth-of-field microscope observation of final institute transfer organization
Figure is as shown in Figure 3.
Claims (3)
1. a kind of high guarantor's type transfer method of PDMS structure, which comprises the steps of:
Step 1: the silicon template (2) of PDMS structure to be transferred is prepared；
Step 2: production PDMS transfer layer (5)；Specifically include following sub-step:
Sub-step one: preparation PDMS blanket layer (3)；
Sub-step two: PDMS blanket layer (3) prepared by sub-step one and a culture dish are put into vitreous evacuated container, taken out
Vacuum, then by intake valve toward injection this inert gas of nitrogen in cabinet until inside and outside air pressure balance；Cabinet is opened rapidly
And silicon fluoride solution is dripped into culture dish, then close cabinet rapidly and carries out vacuum pumping immediately, a period of time is stood,
It is taken out after PDMS blanket layer (3) surface deposited one layer of silicon fluoride；Nitrogen during this is that prevent will as protection gas
The silicon fluoride oxidation deactivation of instillation；
Sub-step three: by sub-step bifluoride treated PDMS blanket layer (3) is put into keep the temperature a period of time in insulating box after take
Out；The process is to make silicon fluoride layer (4) at it to complete the molecule of silicon fluoride layer (4) and PDMS blanket layer (3) surface and assemble
It is more stable on surface to retain；
So far, the production of PDMS transfer layer (5) is completed；
Step 3: along the PDMS solution of silicon template (2) center of the step 1 slowly quasi- amount of examination drop, to it from face center toward surrounding
It scatters, slowly flows into each structural cavities, it is desirable that PDMS solution does not spill over silicon wafer template surface with exterior domain；
Step 4: the PDMS transfer layer (5) made using step 2, being placed in silicon template (2) in step 3 has the one of PDMS structure
Face uniformly applies pressure, is put into after solidifying in insulating box and takes out, then removes silicon template (2), each on such silicon template (2)
PDMS structure in structural cavities is transferred on PDMS transfer layer (5) with regard to guarantor's type；Specifically include following sub-step:
Sub-step one: one piece of clean quartz glass plate (6) is taken, one piece and used silicon wafer mold are fixed in region in its center
The silicon template (2) of comparable size；
Sub-step two: one piece of clean quartz glass plate (6), four pieces of organic glass cushion blocks (8), a solid flexible rubber are separately taken
(7), four binder clips are enclosed, silicon template (2) are fixed on quartz glass plate (6) centre of surface position, by solid flexible rubber circle
(7) it is placed on the quartz glass plate (6) of sub-step one and is surrounded an open cylindrical cavity, organic glass cushion block (8) is placed on
Four positions of solid flexible rubber circle (7), then by other one piece of quartz glass plate (6) with the nethermost quartz glass of face
The direction of plate (6) is covered on composition high precision silicon template loading mold (9) above and prepares chamber II, then with binder clip along four
Uniformly step up to fix in direction；
Sub-step three: prepared toward the high precision silicon template loading mold (9) that sub-step two obtains poured into chamber II it is proportioned
PDMS solution (10) is then placed in solidification in insulating box；PDMS high precision silicon template loading mold (9) is integrally taken after being cured
Out；Silicon template (2) is put into the high precision silicon template loading mold (9), so that silicon template (2) surface and high precision silicon template dress
It carries mold (9) upper surface and keeps concordant.
2. a kind of high guarantor's type transfer method of PDMS structure as described in claim 1, which is characterized in that the step 1 includes
Following sub-step:
Sub-step one: silicon wafer mask plate is prepared；
Sub-step two: photoetching and dry etching are carried out to monocrystalline silicon (1) with mask plate prepared by sub-step one, wait turn needed for obtaining
Move the silicon template (2) of PDMS structure.
3. a kind of high guarantor's type transfer method of PDMS structure as described in claim 1, which is characterized in that the step 2 neutron
The more excellent scheme of step 2 are as follows: mold I is prepared by production PDMS transfer layer (5), then by proportioned PDMS and admittedly
After agent is vacuum-treated, pours into PDMS transfer layer mold I and realized after solidification；The production PDMS transfer layer preparation
The detailed process of mold I are as follows: take two pieces of clean quartz glass plates (6), four pieces of organic glass cushion blocks (8), one it is solid
Solid flexible rubber circle (7) is placed on one of quartz glass plate (6) and surrounds by flexible rubber circle (7), four binder clips
Organic glass cushion block (8) is placed on four positions of rubber ring (7) by one open cylindrical cavity, then by other one piece quartzy glass
Glass plate (6) is covered on the direction of the nethermost quartz glass plate of face (6) and forms PDMS transfer layer above and prepare mold cavity I,
Then uniformly step up to fix along four direction with binder clip.
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