CN105478022B - Miillpore filter preparation method based on Parylene - Google Patents
Miillpore filter preparation method based on Parylene Download PDFInfo
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- CN105478022B CN105478022B CN201510950115.1A CN201510950115A CN105478022B CN 105478022 B CN105478022 B CN 105478022B CN 201510950115 A CN201510950115 A CN 201510950115A CN 105478022 B CN105478022 B CN 105478022B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/72—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, not provided for in a single one of the groups B01D71/46 - B01D71/70 and B01D71/701 - B01D71/702
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0023—Organic membrane manufacture by inducing porosity into non porous precursor membranes
- B01D67/0032—Organic membrane manufacture by inducing porosity into non porous precursor membranes by elimination of segments of the precursor, e.g. nucleation-track membranes, lithography or laser methods
- B01D67/0034—Organic membrane manufacture by inducing porosity into non porous precursor membranes by elimination of segments of the precursor, e.g. nucleation-track membranes, lithography or laser methods by micromachining techniques, e.g. using masking and etching steps, photolithography
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- Manufacturing & Machinery (AREA)
- Filtering Materials (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The miillpore filter preparation method based on Parylene that the invention discloses a kind of is related to the technical field of membrane for being used for separating technology or equipment characterized by material.The method includes the preparation of substrate disk, Parylene preparation, metal layer preparation, the photoetching of micropore figure, development operation, metal micro-holes preparation, photoresist removal, the removal of dry etching miillpore filter, metal layer, miillpore filter preparations.Miillpore filter aperture 3um-50um of the invention, thickness 0.1um-100um are carried out under room temperature environment, dry process preparation, easy to operate, at low cost, fabrication cycle is short, and thermal stability and chemical stability are good, uniformity is good, and chemical toxicity and bio-toxicity are qualified, and no medium falls off, applied widely.
Description
Technical field
The present invention relates to technical field of membrane more particularly to a kind of bases for being used for separating technology or equipment characterized by material
In the miillpore filter preparation method of Parylene.
Background technique
Miillpore filter is that high molecular polymer or inorganic matter manufactured one kind under the conditions of special process are resistance to various organic molten
The sieve type precision filter material of agent, in application of membrane separation technology, miillpore filter is a kind of most wide film kind of application range, can be with
Separation, purification, rich particles, cell, foreign matter, floating dust, aerosol, are widely used in medical and health, biology in liquid phase, gas phase
The departments such as chemistry, microelectronics industry, environmental protection.
Miillpore filter is different according to the target property to be filtered, and the filter membrane of unlike material and different size can be selected, existing
There is filter membrane material to be generally divided into: cellulose mixture film, nylon membrane, PTEE film, pvdf membrane, cellulose nitrate ester film, glass fibers
Tie up film, poly (ether sulfone) film, polypropylene screen, polycarbonate membrane and inoranic membrane.Preparation process is often complex, and due to itself spy
Property, there are preparation process environmental pollution, film-formation result is poor, application field is single a series of problems, such as.
Parylene film be a kind of unbranched, highly crystalline, molecular weight be more than 500,000 paraxylene polymer.According to
The difference of molecular structure, Parylene can be divided into the multiple types such as N-type, c-type, D type, HT type, and the main distinction is to take on molecule
For base difference, the difference of molecular formula also determines that its thermal stability and insulation performance etc. are different.Wherein, c-type is poly- to two
Toluene (Parylene C) film coating is current most popular one kind.Parylene film has moisture-proof, insulation, corrosion resistant
Erosion, biocompatibility, pin-free coating, good mechanical performance and thermal stability, for its unique physical characteristic and electricity
Characteristic, Parylene is common at present is used as microstructured layers, lubricant coating, protection corrosion-inhibiting coating, dielectric isolation layer and dielectric material,
The fields such as Aeronautics and Astronautics, military project, microelectronics, semiconductor, medical treatment, text guarantor are widely used in, but are being used for miillpore filter preparation side
Face is there is not yet relevant report.
Summary of the invention
The miillpore filter preparation method based on Parylene that technical problem to be solved by the invention is to provide a kind of, it is described
Method carries out under room temperature environment, and dry process preparation, easy to operate, at low cost, fabrication cycle is short, and thermal stability and chemistry are steady
Qualitative good, uniformity is good, and chemical toxicity and bio-toxicity are qualified, and no medium falls off, applied widely.
In order to solve the above technical problems, the technical solution used in the present invention is: a kind of micropore filter based on Parylene
Membrane preparation method, it is characterised in that include the following steps:
1) Parylene film preparation: Parylene film is prepared on silicon wafer surface；
2) prepared by metal layer: deposition prepares metal layer on Parylene film, the metal mask for etching as micropore；
3) micropore figure photoetching: with micropore mask plate in Parylene film upper surface photoetching micropore figure, the exposure mask packet
Include non-photo-sensing area and photosensitive area；
4) development operation: after disk develops in developer solution, removing photosensitive area photoresist, forms band glue region and adhesive-free area
The micropore figure in domain；
5) prepared by metal micro-holes: disk is immersed in corrosive liquid, removes the metal layer under unglazed photoresist region, forms micropore
Shape metal mask；
6) photoresist removes: disk impregnates in acetone, removes photomask surface glue；
7) dry etching miillpore filter: the exposure mask etched using micropore shape metal mask as this controls the aperture of micropore
Size etches Parylene film based on deep reaction ion etching principle, keeps the Parylene under no metal mask region complete
Etching is clean, forms miillpore filter；
8) metal layer removes: disk is immersed in corrosive liquid, removes surface metal-layer；
9) prepared by miillpore filter: disk is immersed in potassium hydroxide solution, peels off miillpore filter naturally from disk surfaces,
Finally obtain miillpore filter.
A further technical solution lies in: the method further includes the steps that substrate disk prepares before step 1): with
The substrate that clean silicon wafer is prepared as miillpore filter, the upper surface of silicon wafer are burnishing surface.
A further technical solution lies in: the step 1) specifically: chemical vapor deposition principle is utilized, in silicon wafer table
For wheat flour for Parylene film, Parylene film thickness is 0.1um-100um；Deposition process can be divided into three steps, under vacuum conditions,
Solid feed is sublimed into gaseous state at a temperature of 100-150 DEG C；Dimer gas enters cracking chamber, at a temperature of 600-700 DEG C, two
The molecular link of aggressiveness is disconnected, and is cracked into the monomer with reactivity；Vacuum of the last Parylene gaseous monomer in room temperature
It deposits and polymerize in settling chamber, form Parylene film on the surface of silicon wafer.
A further technical solution lies in: in the step 2: the metal layer is aluminum metal layer, with a thickness of 1000-
2000Å。
A further technical solution lies in: in the step 3): thick just in layer on surface of metal coating 4000-6000
Property photoresist, for disk in 110-120 DEG C of baking 2min-3min, time for exposure 5s-6s, the exposure mask includes that chromium is non-before photoetching
Photosensitive area and glass photosensitive area.
A further technical solution lies in: developing time 40s-45s in the step 4), disk is in 110-120 after development
DEG C baking 10 min-15min.
A further technical solution lies in: corroded in the step 5) and step 8) using aluminium corrosive liquid, by volume
Phosphoric acid than 16:2:1: deionized water: nitric acid solution is made into, 50 DEG C heating water bath 1 hour, wherein step 5) metal micro-holes system
Standby, 15 s -30s of etching time, step 8) removes metal layer, etching time 2min-3min.
A further technical solution lies in: disk impregnates the time in acetone for 15-20min in the step 6).
A further technical solution lies in: in the step 7), reaction gas of the oxygen as etching Parylene is used
Dijection frequency source RF1 and RF2 control etching process, and wherein RF1 radio frequency source generates plasma for causing oxygen gas glow discharge
Body, RF2 radio frequency source are used to provide the energy for accelerating etching to plasma, and etching process includes oxygen plasma to Parylene
Physical bombardment and oxygen and Parylene chemical reaction, ultimately form microcellular structure；By adjusting operating pressure, reaction
Temperature and RF2 RF source power effectively change the etch rate and micropore sidewall profile of Parylene, and then control micropore size
Size.
A further technical solution lies in: in the step 9): disk is immersed in 1min-2min in potassium hydroxide solution,
Potassium hydroxide solution for peeling off miillpore filter is volume ratio=1:20 potassium hydroxide: deionized water solution.
The beneficial effects of adopting the technical scheme are that the method carries out under room temperature environment, dry method work
Skill preparation, easy to operate, at low cost, fabrication cycle is short, and thermal stability and chemical stability are good, and uniformity is good, chemical toxicity and
Bio-toxicity is qualified, and no medium falls off.The miillpore filter made by the method has different pore size specification, different pore size
Distribution, can simple and effective progresss cell separation, the filtering of organic/inorganic solvent can be widely applied to biomedical, industry and gives birth to
The multiple fields such as production, food safety, energy environment protection.
Detailed description of the invention
Fig. 1-10 is the procedure structure schematic diagram of the filter membrane of the method preparation through the invention；
Figure 11 is the silicon wafer schematic diagram with miillpore filter of the method preparation through the invention；
Figure 12 is the miillpore filter schematic diagram of the method preparation through the invention；
Figure 13 is the miillpore filter sectional view of the method preparation through the invention；
Wherein: 1, silicon wafer 2, Parylene film 3, metal layer 4, non-photo-sensing area 5, photosensitive area 6, photoresist 7, band glue region
8, glue free spaces 9, miillpore filter.
Specific embodiment
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
The miillpore filter preparation method based on Parylene that the invention discloses a kind of, includes the following steps:
Substrate disk prepares: the substrate prepared using clean silicon wafer 1 as miillpore filter, Parylene film to be deposited
Silicon face is burnishing surface, as shown in Figure 1；
Parylene film preparation: using chemical vapor deposition process, Parylene film is prepared on silicon wafer 1, such as Fig. 2 institute
Show, raw material is paraxylene cyclodimerization body.Deposition process can substantially be divided into three steps, under vacuum conditions, 100-150 DEG C of temperature
It is lower that solid feed is sublimed into gaseous state；Dimer gas enters cracking chamber, at a temperature of 600-700 DEG C, the molecular link of dimer
It is disconnected, is cracked into the monomer with reactivity；Last Parylene gaseous monomer deposits in the vacuum deposition chamber of room temperature
And polymerize, Parylene film 2 is formed on the surface of silicon wafer.
Metal layer preparation: it is preferred, it is based on electron beam evaporation principle, is melted with the electron beam of high-energy focusing and evaporates aluminium
Material, prepares aluminum metal layer 3 in the upper surface of Parylene film 2, as shown in figure 3, the aluminum metal layer of preparation is with a thickness of 1000-
2000, this step process provides exposure mask for the preparation of subsequent miillpore filter.
Micropore figure photoetching: 4000-6000 positive photoresists 6 are coated on aluminum metal layer surface, then at 110 DEG C-120
DEG C baking 2-3min, with micropore mask plate photoetching micropore figure, ultraviolet exposure 5s -6s keeps glass photosensitive area photoresist solvable
In developer solution, as shown in Figure 4.
Development operation: above-mentioned disk is impregnated in developer solution, and develop 40s-45s, removes the photoresist of glass photosensitive area
6, disk forms micropore figure, as shown in Figure 5 in 110 DEG C of -120 DEG C of baking 10-15min after development.
Metal micro-holes preparation: disk is immersed in aluminium corrosive liquid, and wherein aluminium corrosive liquid volume proportion is phosphoric acid: deionization
Water: nitric acid=16:2:1；Before use, by aluminium corrosive liquid as 50 DEG C heating water bath 1 hour, stir evenly, be put into corrosion corrosion
In the process, metal removal situation in micropore is observed, clean rear taking-up is corroded, bath drying obtains micropore shape metal mask, such as figure
Shown in 6.
Photoresist removal: disk is impregnated in acetone, can effectively remove photoresist, waits about 15-20min photoresist complete
After being dissolved in acetone entirely, disk 10-15min is impregnated using ethyl alcohol, removes remained on surface acetone, then drying of washing by water, as shown in Figure 7.
Dry etching miillpore filter: being based on deep reaction ion etching principle (DRIE), etches under metal mask
Parylene film, etching gas are oxygen, are controlled using dijection frequency source (RF1 and RF2), wherein after the pressurization of RF1 radio frequency source, energy
Coupling generates alternating magnetic field, and electronics is spinned movement under magnetic fields, causes oxygen gas glow discharge, generates with electrochondria
The plasmas such as son, reactive radical species, atom；RF2, with RF1 radio frequency source Phase synchronization, makes plasma for providing bias voltage
Bias also reaches highest when density highest, it is ensured that the performance of high-density plasma corrasion achievees the effect that etching, RF2
The utilization of bias radio frequency source makes plasma act perpendicularly to the surface Parylene to greatest extent, greatly improves hanging down for micropore
Straight degree, while the Parylene under effective protection metal mask is not etched, etching process includes that physical reactions and chemistry are anti-
It answers, physical reactions are physical bombardment of the oxygen plasma to Parylene, reach removal effect, while oxygen can be with Parylene
It chemically reacts, generates volatilizable gas, achieve the effect that removal, the continuous action of two kinds of reactions makes no metal mask
Micro-porous area Parylene layers of etching of covering is clean, ultimately forms micropore, as shown in Figure 8.
Optionally, can effectively change by adjusting operating pressure, reaction temperature and the RF2 RF source power in technical process
Parylene etch rate and micropore sidewall profile, and then control micropore size size.
Metal layer removal: corroding corrosion metal mask using aluminium, and disk is soaked into 2-3min in corrosive liquid, waits table
Face metal corrodes completely fall off after, take out bath drying, as shown in Figure 9.
Miillpore filter preparation: disk is put into potassium hydroxide solution, and wherein volume ratio is potassium hydroxide: deionized water=
1:20, after impregnating 1-2min, Parylene miillpore filter falls off naturally from silicon chip surface, after bath, takes out miillpore filter, natural
It air-dries, final preparation forms miillpore filter, as shown in Figure 10.
Figure 11 is the silicon wafer schematic diagram with miillpore filter of the method preparation through the invention.
Figure 12 is the miillpore filter schematic diagram of the method preparation through the invention.
Figure 13 is the miillpore filter sectional view of the method preparation through the invention.
The method carries out under room temperature environment, and dry process preparation, easy to operate, at low cost, fabrication cycle is short, and heat is steady
Qualitative and chemical stability is good, and uniformity is good, and chemical toxicity and bio-toxicity are qualified, and no medium falls off.By the method system
The miillpore filter of work, have different pore size specification, different pore size be distributed, can simple and effective progress cell separation, organic/inorganic
The filtering of solvent can be widely applied to the multiple fields such as biomedicine, industrial production, food safety, energy environment protection.
Claims (7)
1. a kind of miillpore filter preparation method based on Parylene, it is characterised in that include the following steps:
1) Parylene film (2) Parylene film preparation: are prepared on silicon wafer (1) surface；
2) prepared by metal layer: deposition prepares metal layer (3) on Parylene film (2), and the metal for etching as micropore is covered
Film；
3) micropore figure photoetching: the metal layer lithography micropore figure with micropore mask plate in Parylene film upper surface, it is described micro-
Hole mask plate includes non-photo-sensing area (4) and photosensitive area (5), wherein the metal with micropore mask plate in Parylene film upper surface
Layer photoetching micropore figure includes: in the layer on surface of metal coating positive photoresist of silicon wafer, to the silicon for being coated with positive photoresist
Disk is toasted, is exposed by micropore mask plate to the silicon wafer after baking；
4) development operation: silicon wafer develops in developer solution, and after development, removes the photoresist (6) of photosensitive area, forms band glue
The micropore figure in region (7) and glue free spaces (8)；
5) prepared by metal micro-holes: silicon wafer is immersed in corrosive liquid, is removed the metal layer under glue free spaces, is formed micro- perforated metal
Exposure mask；
6) photoresist removes: silicon wafer impregnates in acetone, removes the photoresist (6) on surface；
7) dry etching miillpore filter: the exposure mask etched using removing the micropore shape metal mask after photoresist as this, control
The aperture size of micropore is made under no metal mask region based on deep reaction ion etching principle etching Parylene film (2)
Parylene is clean by complete etching, forms miillpore filter；
8) metal layer removes: silicon wafer is immersed in corrosive liquid, removes surface metal-layer；
9) prepared by miillpore filter: silicon wafer is immersed in potassium hydroxide solution, peels off miillpore filter naturally from silicon wafer surface,
Finally obtain miillpore filter (9)；
In the step 9): silicon wafer is immersed in 1min-2min in potassium hydroxide solution, for peeling off the hydroxide of miillpore filter
Potassium solution is volume ratio=1:20 potassium hydroxide: deionized water solution；
In the step 7), reaction gas of the oxygen as etching Parylene is controlled using dijection frequency source RF1 and RF2 and is etched
Process, wherein RF1 radio frequency source generates plasma, RF2 radio frequency source is used for plasma for causing oxygen gas glow discharge
Body provides the energy for accelerating etching, etching process include oxygen plasma to the physical bombardment and oxygen of Parylene with
The chemical reaction of Parylene, ultimately forms microcellular structure；By adjusting operating pressure, reaction temperature and RF2 RF source power
Effectively change the etch rate and micropore sidewall profile of Parylene, and then controls micropore size size；
In the step 2): the metal layer (3) is aluminum metal layer, with a thickness of
2. the miillpore filter preparation method based on Parylene as described in claim 1, it is characterised in that the method is in step
It is rapid 1) to further include the steps that substrate disk prepares before: the substrate prepared using clean silicon wafer (1) as miillpore filter, silicon circle
The upper surface of piece is burnishing surface.
3. the miillpore filter preparation method based on Parylene as described in claim 1, it is characterised in that the step 1) tool
Body are as follows: utilize chemical vapor deposition principle, prepare Parylene film (2) on silicon wafer (1) surface, Parylene film thickness is
0.1μm-100μm；Deposition process is divided into three steps, under vacuum conditions, by solid feed paraxylene ring at a temperature of 100-150 DEG C
Dimer is sublimed into gaseous state and obtains paraxylene cyclodimerization body gas；Paraxylene cyclodimerization body gas enters cracking chamber,
At a temperature of 600-700 DEG C, the molecular link of paraxylene cyclodimerization body is disconnected, and is cracked into the monomer with reactivity；Finally
Monomer deposits and polymerize in the vacuum deposition chamber of room temperature, and Parylene film is formed on the surface of silicon wafer.
4. the miillpore filter preparation method based on Parylene as described in claim 1, it is characterised in that in the step 3):
It is coated on metal layer (3) surfaceThick positive photoresist, silicon wafer is toasted at 110-120 DEG C before exposing
2min-3min, time for exposure 5s-6s, the exposure mask include chromium non-photo-sensing area and glass photosensitive area.
5. the miillpore filter preparation method based on Parylene as described in claim 1, it is characterised in that in the step 4)
Developing time 40s-45s, disk is in 110-120 DEG C of baking 10min-15min after development.
6. the miillpore filter preparation method based on Parylene as described in claim 1, it is characterised in that the step 5) and
Corroded in step 8) using aluminium corrosive liquid, by the phosphoric acid of volume ratio 16:2:1: deionized water: nitric acid solution is made into, corrosion
Before, aluminium corrosive liquid is placed in 50 DEG C of heating water baths 1 hour, wherein the preparation of step 5) metal micro-holes, etching time 15s-30s, step
Rapid 8) metal layer removal, etching time 2min-3min.
7. the miillpore filter preparation method based on Parylene as described in claim 1, it is characterised in that in the step 6)
Silicon wafer impregnates the time in acetone for 15-20min.
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| CN112516804A (en) * | 2019-09-18 | 2021-03-19 | 无锡华润微电子有限公司 | PM2.5 protective equipment, PM2.5 filtering membrane and preparation method thereof |
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