CN114534647B - Film emulsifying device and manufacturing method thereof - Google Patents
Film emulsifying device and manufacturing method thereof Download PDFInfo
- Publication number
- CN114534647B CN114534647B CN202210002531.9A CN202210002531A CN114534647B CN 114534647 B CN114534647 B CN 114534647B CN 202210002531 A CN202210002531 A CN 202210002531A CN 114534647 B CN114534647 B CN 114534647B
- Authority
- CN
- China
- Prior art keywords
- hole
- photoresist layer
- photoresist
- film
- layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
Abstract
The application provides a film emulsification device and a manufacturing method thereof. The film emulsifying device is used for manufacturing the discrete phase microspheres and comprises a film, a film and a film, wherein the film is provided with a plurality of through hole structures and used for allowing the discrete phase to pass through; the thin film comprises a first photoresist layer and a second photoresist layer, the through hole structure comprises a first through hole arranged on the first photoresist layer and a second through hole arranged on the second photoresist layer, and the second through hole is correspondingly communicated with the first through hole; the thickness of the first photoresist layer is smaller than that of the second photoresist layer, and the size of the first through hole is smaller than that of the second through hole. The thin film is provided with a plurality of through hole structures, wherein the second through holes are correspondingly communicated with the first through holes and used for allowing the discrete phases to pass through; the requirement of thinning the thickness of the film can be met, the film is guaranteed not to be broken when bearing high pressure, and meanwhile, the aperture uniformity on the film is excellent and the size is very small.
Description
Technical Field
The application relates to the field of drug delivery, in particular to a film emulsifying device and a manufacturing method thereof.
Background
Membrane emulsification devices are widely used for microsphere fabrication due to their high throughput, which requires two immiscible fluids, such as a continuous phase and a discrete phase. As shown in FIG. 1, the discrete phases flow out through the pores of the film and interact with the continuous phase to form microspheres under the shear forces generated. The continuous phase may be formed by means of a syringe pump, stirring, shaking, etc. The microsphere size D _ D is determined in large part by the membrane pore size D _ p, and typically D _ D is about 2 to 10 times larger than D _ p. Therefore, in order to obtain small-sized microspheres, the pore size of the membrane needs to be minimized. The thickness of the film should be reduced correspondingly under the limitation of the processing technology of the aperture with the high aspect ratio, otherwise, the small aperture film cannot be obtained. The reduction in film thickness will result in the film not being able to withstand high pressures and thus breaking. There are two ways to solve this problem: firstly, the thickness of the film is increased, but as mentioned above, the aperture cannot be reduced due to the limitation of the processing technology; secondly, the thin film is made of a high-strength and high-ductility material, such as a Shirasu Porous Glass (SPG) novel inorganic film (SPG science and technology Co., japan), which is widely used at present. In the production process of the SPG film, volcanic ash, glass and lime are subjected to boric acid forming at 1350 ℃, and then are heated to about 700 ℃ to produce glass containing O.B _2O _3particles with good uniformity. The glass is dissolved in acid, and CaO.B _2O _3particles are dissolved by the acid solution, thereby forming porous glass with a pore diameter of 0.1-20 μm and excellent pore diameter uniformity. However, SPG films have two disadvantages. Firstly, because the structure of hole is mostly the distortion irregular structure, is easily contaminated by the phase that disperses, and secondly this membrane price is comparatively expensive, especially compares with present silicon membrane widely used in microsystem, and the cost is higher.
Disclosure of Invention
The invention aims to provide a film emulsifying device and a manufacturing method thereof, which are used for reducing the thickness of a film and ensuring that the film is not broken when the film is subjected to high pressure, and meanwhile, the aperture uniformity on the film is excellent and the size is small.
In order to achieve the above objects, one embodiment of the present invention provides a membrane emulsification device for making microspheres with discrete phases, comprising a membrane having a plurality of through hole structures for passing the discrete phases; the thin film comprises a first photoresist layer and a second photoresist layer, the through hole structure comprises a first through hole arranged on the first photoresist layer and a second through hole arranged on the second photoresist layer, and the second through hole is correspondingly communicated with the first through hole; the thickness of the first photoresist layer is smaller than that of the second photoresist layer, and the size of the first through hole is smaller than that of the second through hole.
Furthermore, the first through hole and the second through hole are both square, and the first through hole and the second through hole are coaxially arranged in the direction perpendicular to the film.
Furthermore, the cross section of the first through hole and the cross section of the second through hole are both square, and the side of the first through hole and the side of the second through hole are arranged in parallel; the length ratio of the side of the cross section of the first through hole to the side of the cross section of the second through hole is 1:20 to 1:10.
further, the thickness of the first photoresist layer is equal to the length of the side of the cross section of the first through hole, and the thickness of the second photoresist layer is equal to the length of the side of the cross section of the second through hole.
Further, the membrane emulsification device further comprises: a discrete phase feed connected to one side of the membrane for controlling the flow of the discrete phase supplied to the membrane; and a magnetic stirrer to provide a shear force to the discrete phases, wherein the direction of the shear force is perpendicular to the direction of flow of the discrete phases.
Further, the film is in sealed connection with the discrete phase feeding device; and a container is arranged on the magnetic stirrer and used for placing the continuous phase and containing the manufactured discrete phase microspheres.
The application also provides a manufacturing method of the film emulsifying device, which comprises the steps of manufacturing a film; the step of manufacturing the film comprises: manufacturing a metal layer on a glass substrate, coating photoresist on the metal layer and carrying out patterning treatment to form a first photoresist layer, wherein a first through hole is formed in the first photoresist layer; etching the metal layer and reserving the metal layer below the first photoresist layer; coating photoresist on the glass substrate and the first photoresist layer and carrying out patterning treatment to form a second photoresist layer, wherein a second through hole is formed in the second photoresist layer and is correspondingly communicated with the first through hole; the size of the first through hole is smaller than that of the second through hole; and etching to remove the glass substrate and the residual metal layer.
Further, the step of coating photoresist on the metal layer and patterning to form a first photoresist layer comprises: arranging a first mask plate above the coated photoresist, wherein the first mask plate is provided with a first shading area and a first light transmitting area, the shape of the first light transmitting area is the cross section of a first through hole, the photoresist corresponding to the first shading area is washed and removed by a developer after the photoresist is exposed, baked and solidified by laser, and a first photoresist layer is formed after oxygen plasma cleaning; further, the step of coating photoresist on the glass substrate and the first photoresist layer and patterning to form a second photoresist layer comprises: set up the second mask plate in the photoresist top of coating, the second mask plate is equipped with second shading area and second printing opacity district, the shape in second printing opacity district is the cross section of second through-hole, through laser exposure and toast the solidification behind the photoresist will correspond the back is washed to the developer for the photoresist in second shading area and is got rid of, washes with isopropyl alcohol and carries out the drying with nitrogen gas after and form second photoresist layer.
Furthermore, the material of the metal layer comprises chromium, and the glass substrate is removed by etching with hydrofluoric acid.
Further, before the etching to remove the glass substrate and the remaining metal layer, the method further comprises: and sealing and attaching vent pipes of the discrete phase feeding devices on the second photoresist layer around the second through holes.
The invention has the beneficial effects that the film emulsifying device and the manufacturing method thereof are provided, the film with the first photoresist layer and the second photoresist layer is manufactured in a mode of removing the glass substrate and the metal layer by etching, so that the film is provided with a plurality of through hole structures, wherein the second through holes are correspondingly communicated with the first through holes, and are used for allowing discrete phases to pass; the requirement of thinning the thickness of the film can be met, the film is guaranteed not to be broken when bearing high pressure, and meanwhile, the aperture uniformity on the film is excellent and the size is very small.
Drawings
The following detailed description of the embodiments of the present application, taken in conjunction with the accompanying drawings, presents the technical solutions and other advantages of the present application.
FIG. 1 is a schematic diagram of the prior art of microsphere formation in a continuous phase by flowing a discrete phase through a thin film pore.
Fig. 2 is a top view of a film in the film emulsifying apparatus provided in the embodiment of the present application.
Fig. 3 isbase:Sub>A cross-sectional view atbase:Sub>A-base:Sub>A in fig. 2.
Fig. 4 is a schematic structural diagram of a method for manufacturing a thin film emulsification device according to an embodiment of the present disclosure when a first photoresist layer is formed by exposing a photoresist.
Fig. 5 is a schematic structural diagram of a method for manufacturing a thin film emulsification device according to an embodiment of the present disclosure when a second photoresist layer is formed by coating a photoresist.
Fig. 6 is a schematic structural diagram of a process of forming a second photoresist layer by coating and exposing a photoresist in the method for manufacturing a thin film emulsification device according to the embodiment of the present application.
Fig. 7 is a schematic structural diagram illustrating a through hole structure of a thin film formed in a method for manufacturing a thin film emulsification apparatus according to an embodiment of the present disclosure.
Fig. 8 is a schematic structural view of a vent pipe of a discrete phase feeding device attached to a film in a film emulsifying device according to an embodiment of the present application.
Fig. 9 is a schematic structural diagram of a film emulsifying apparatus provided in an embodiment of the present application.
Fig. 10 is a structural schematic diagram of a use state of the film emulsifying device according to the embodiment of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly and include, for example, fixed or removable connections or integral connections; may be mechanically, electrically or may be in communication with each other; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
In this application, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may comprise direct contact of the first and second features, or may comprise contact of the first and second features not directly but through another feature in between. Also, the first feature being "on," "above" and "over" the second feature includes the first feature being directly on and obliquely above the second feature, or merely indicating that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature includes the first feature being directly under and obliquely below the second feature, or simply meaning that the first feature is at a lesser elevation than the second feature.
Specifically, referring to fig. 2 to 10, the present application provides a thin film emulsification device for manufacturing discrete phase microspheres, which includes a thin film 10 having a plurality of through hole structures for passing through discrete phases. The thin film 10 comprises a first photoresist layer 11 and a second photoresist layer 12, the through hole structure comprises a first through hole 1 arranged on the first photoresist layer 11 and a second through hole 2 arranged on the second photoresist layer 12, and the second through hole 2 is correspondingly communicated with the first through hole 1; the thickness of the first photoresist layer 11 is smaller than that of the second photoresist layer 12, and the size of the first through hole 1 is smaller than that of the second through hole 2.
Further, the first through hole 1 and the second through hole 2 are both square, and the first through hole 1 and the second through hole 2 are coaxially arranged in a direction perpendicular to the film 10.
Further, the cross section of the first through hole 1 and the cross section of the second through hole 2 are both square, and the side of the first through hole 1 and the side of the second through hole 2 are arranged in parallel; the length ratio of the side of the cross section of the first through hole 1 to the side of the cross section of the second through hole 2 is 1:20 to 1:10.
further, the thickness of the first photoresist layer 11 is equal to the length of the side of the cross section of the first through hole 1, and the thickness of the second photoresist layer 12 is equal to the length of the side of the cross section of the second through hole 2. Specifically, the thickness of film 10 is 21um, the thickness of first photoresist layer 11 is 1um, the length on the limit of the cross section of first through-hole 1 is 1um, the thickness of second photoresist layer 12 is 20um, the length on the limit of the cross section of second through-hole 2 is 20um.
Referring to fig. 10, further, the membrane emulsification apparatus 100 further comprises: a discrete phase feeding means 20 connected to one side of the thin film 10 for controlling a flow rate of the discrete phase supplied to the thin film 10; and a magnetic stirrer 30 to provide a shear force to the discrete phases, wherein the direction of the shear force is parallel to the surface of the thin film 10 and perpendicular to the direction of flow of the discrete phases.
Referring to fig. 10, further, the film 10 is hermetically connected to the discrete phase feeding device 20; a container 40 is disposed on the magnetic stirrer 30 for holding the continuous phase and containing the prepared discrete phase microspheres.
Based on the membrane emulsification device, the present application also provides a method for manufacturing the membrane emulsification device 100, which includes the steps of manufacturing a membrane 10; the step of manufacturing the film 10 includes: manufacturing a metal layer 14 on a glass substrate 13, coating photoresist on the metal layer 14 and performing patterning treatment to form a first photoresist layer 11, wherein a first through hole 1 is formed in the first photoresist layer 11; etching the metal layer 14, and reserving the metal layer 14 below the first photoresist layer 11; coating photoresist on the glass substrate 13 and the first photoresist layer 11 and performing patterning treatment to form a second photoresist layer 12, wherein a second through hole 2 is formed in the second photoresist layer 12, and the second through hole 2 is correspondingly communicated with the first through hole 1; the size of the first through hole 1 is smaller than that of the second through hole 2; and etching to remove the glass substrate 13 and the remaining metal layer 14.
Further, the step of coating a photoresist on the metal layer 14 and patterning to form the first photoresist layer 11 includes: arranging a first mask plate 21 above the coated photoresist, wherein the first mask plate 21 is provided with a first shading area 211 and a first light transmitting area 212, the shape of the first light transmitting area 212 is the cross section of the first through hole 1, the photoresist corresponding to the first shading area 211 is washed and removed by developer after the photoresist is exposed, baked and solidified by laser, and a first photoresist layer 11 is formed after oxygen plasma cleaning; further, the step of coating photoresist on the glass substrate 13 and the first photoresist layer 11 and patterning to form the second photoresist layer 12 includes: the second mask plate 22 is arranged above the coated photoresist, the second mask plate 22 is provided with a second shading area 221 and a second light transmitting area 222, the second light transmitting area 222 is in the shape of the cross section of the second through hole 2, the photoresist is exposed through laser, baked and solidified, then the photoresist corresponding to the second shading area 221 is washed and removed by using a developer, and then the photoresist is washed by using isopropanol and dried by using nitrogen to form the second photoresist layer 12.
Further, the material of the metal layer 14 includes chromium, and the glass substrate 13 is removed by etching with hydrofluoric acid.
Further, before the etching to remove the glass substrate 13 and the remaining metal layer 14, the method further includes: and the vent pipe of the discrete phase feeding device 20 is hermetically attached to the second photoresist layer 12 by AB glue 15 around the second vent hole 2.
The invention manufactures the film 10 with the first photoresist layer 11 and the second photoresist layer 12 by etching to remove the glass substrate 13 and the metal layer 14, so that the film 10 has a plurality of through hole structures with the second through holes 2 correspondingly communicated with the first through holes 1 for passing discrete phases; the requirement of thinning the thickness of the film 10 can be met, the film is guaranteed not to be broken when the film is subjected to high pressure, and meanwhile, the aperture uniformity of the film 10 is excellent and the size is small.
The principles of this application are described in detail below by describing specific embodiments thereof in detail.
As previously mentioned, the film 10 is required to meet two basic requirements, the fabrication of small size microspheres and the ability to withstand pressures of about 120kPa, which are met by the multi-layer design proposed in this patent, the basic structure of which is shown in FIG. 2. The film 10 is composed of two layers of structures, wherein the upper layer of structure is a square hole with the side length and the depth of 20 mu m, and the lower layer of structure is a square hole with the side length and the depth of 1 mu m. Fig. 3 shows the cross-sectional dimensions of the porous membrane 10, and it can be seen that the upper layer pore structure of the membrane 10 can meet the requirement of the membrane 10 for pressure resistance, and the lower layer pore structure can meet the requirement of making small-sized microspheres. Due to the multi-layer structure design of the film 10, the manufacturability of the film in terms of the aspect ratio is also greatly improved (the upper layer structure is 20.
When the thin film 10 is manufactured, the photoresist adopts SU-8 2000 series, and the SU-8 2000 series is suitable for thick films with the thickness of 0.5 to more than 200 mu m and the high aspect ratio of more than 10: 1. The method of making the film 10 is as follows:
(a) Sputtering of chromium
A glass substrate 13 having a thickness of 100 μm was sputtered with a layer of chromium having a thickness of 120nm to form a metal layer 14. Since the glass substrate 13 and the SU-8 are both transparent, the chrome layer mainly serves for hole observation and alignment of the alignment marks.
(b) SU-8 spin coating (1 μm)
SU-8 2001 was spin-coated on the chromium layer at 1500 revolutions per minute (rpm) for 3 seconds(s) and then at 4000rpm for 30s. Followed by soft baking at 95 ℃ for 1 minute.
(c) Mark alignment
The mask plate 21 is aligned by two cross mark alignment methods.
(d) Exposure to light
The resulting photoresist was exposed to light with a laser power of 100mW and a wavelength of 355nm. As shown in fig. 4, fig. 4 is a schematic structural diagram of a method for manufacturing a thin film emulsification apparatus according to an embodiment of the present disclosure when exposing a photoresist to form a first photoresist layer 11.
(e) Post Exposure Bake (PEB)
The photoresist was baked at 95 ℃ for 1 minute.
(f) Development
The photoresist was soaked in developer (propylene glycol methyl ether acetate, PGMEA) for 1 minute, then rinsed with isopropyl alcohol (IPA) for 30 seconds, and finally with nitrogen (N) 2 ) Drying is carried out. The opaque region corresponding to the photoresist is removed to obtain a first through hole 1 with an aperture of 1 × 1 μm 2 The first photoresist layer 11.
(g) Oxygen-plasma deslagging and cleaning for 5 minutes.
(h) Boundary chromium etch
Chromium outside the porous region needs to be removed. The chromium outside the area is soaked in the etching solution for 45 seconds and then washed clean by distilled water. It is noted that this step is only to remove the border chromium metal layer 14.
(i) SU-8 spin coating (20 μm)
SU-8 2025 was spin coated on the glass substrate 13 and the first photoresist layer 11 at 500rpm for 1 second. Then, the spin speed was accelerated to 4000rpm for 10 seconds and held for 30 seconds. The photoresist was then soft baked at 65 ℃ for 1 minute, then the temperature was raised to 95 ℃ for 5 minutes. As shown in fig. 5, fig. 5 is a schematic structural diagram of a method for preparing a thin film emulsification apparatus according to an embodiment of the present disclosure when a second photoresist layer 12 is formed by coating a photoresist.
(j) Mark alignment
The mask 21 is used to align two SU-8 film layers with two cross marks. The cross mark on the first SU-8 film layer is completely covered by the cross mark on the second SU-8 film layer. At this time, the prepared second through hole 2 and the first through hole 1 can be correspondingly communicated.
(k) Exposure method
The resulting photoresist was exposed to light with a laser power of 100mW and a wavelength of 355nm. As shown in fig. 6, fig. 6 is a schematic structural diagram of a second photoresist layer 12 formed by coating and exposing a photoresist in the method for manufacturing a thin film emulsification device according to the embodiment of the present application.
(l) Post Exposure Bake (PEB)
The photoresist was baked at 65 ℃ for 1 minute, then the temperature was raised to 95 ℃ and baked for 5 minutes.
(m) development
The photoresist was soaked in developer (propylene glycol methyl ether acetate, PGMEA) for 4 minutes, then rinsed with isopropyl alcohol (IPA) for 30 seconds, and finally with nitrogen (N) 2 ) Drying is carried out. The opaque region corresponding to the photoresist is removed to obtain a second via 2 with a 20 × 20 μm aperture 2 Of the second photoresist layer 12. As shown in fig. 7, fig. 7 is a schematic structural diagram of a through hole structure of a film formed in the method for preparing a film emulsification apparatus according to the embodiment of the present application.
(n) bonding to an acrylonitrile-butadiene-styrene copolymer (ABS) tube
(o) removing the glass substrate 13 and the chromium metal layer 14
On the first day, the glass substrate 13 was immersed in a 5% Hydrofluoric (HF) acid solution for 8 hours. The next day, the glass substrate 13 is again immersed in a 5% hydrofluoric acid solution for 5 hours for completely removing the glass substrate 13. And then, putting the chromium metal layer 14 into a chromium etching solution for 3 to 4 minutes to remove the chromium metal layer 14, cleaning the chromium metal layer by using distilled water, and drying the chromium metal layer by using nitrogen. Three porous films were fabricated in this experiment to test the feasibility of the structure to fabricate microspheres, as shown in fig. 9. Fig. 9 is a schematic structural diagram of a film emulsification device according to an embodiment of the present application.
Fig. 10 is a schematic view showing a structure of a thin film emulsification device according to the present application in a use state. Experiments prove that the film can be used for preparing microspheres with small size and good uniformity under the condition of high discrete phase flow or high stirring speed.
In this test experiment, paraffin oil (all Sigma-Aldrich, USA) containing 2% of span 80 surfactant was used as the continuous phase. The dispersed phase was distilled water. The multilayer structure film is processed in a micro-nano processing laboratory (SyLMAND) of a Canadian light source Center (CLS) by adopting SU-8 2000 series.
A magnetic stirrer (Corning PC 210, corning Inc., USA) was used to provide the shear force. Syringe pumps employ harvard instruments, usa, to control the flow of discrete phases, requiring calibration before use. The syringe used was a 6 ml syringe from Covidien, ireland and the Polytetrafluoroethylene (PTFE) tube used was a 1.34mm tube from Adtech Polymer engineering machinery, uk. Microscope an Olympus IX70 optical inverted microscope from Olympus, japan was used to observe the microsphere formation process. Post-processing software ImageJ software from the national health center was used for analytical measurements of microsphere size. The size of each microsphere is averaged over 5 measurements. The test experiments are all finished in a micro-nano processing laboratory, and the experimental conditions are room temperature (20 +/-2 ℃).
The minimum pressure for the discrete phase to pass through the film smoothly is
Wherein γ is the interfacial tension prior to the continuous and discrete phases; theta is the contact angle of the discrete phase and the film in the continuous phase; d p Is the pore size. In the present study, the interfacial tension γ =3.65 × 10 -3 N.m -1 The contact angle θ of the discrete phase with the film in the continuous phase is assumed to be 0. Therefore, the minimum pressure
From this, the flow rate of the discrete phase was calculated to be about 5. Mu.l.h -1 . In the test experiment, the flow rate of the discrete phase was set to 10 times the minimum flow rate, which was about 50. Mu.l · h -1 . The stirring speed of the magnetic stirrer was set to 60,80 and 100rpm, respectively. After microsphere formation, 1ml of continuous phase containing microspheres was extracted from the beaker and placed in a clean petri dish for microsphere size observation. The resolution of the microscope used in this experiment is 1 μm, and the post-processing analysis software can reduce the resolution to 0.01 μm by interpolation fitting. White dots suspended in the continuous phase in the beaker are the microspheres produced. Microspheres were produced through the SU-8 film at a stirring speed of 60,80 and 100rpm, respectively. It is understood that an increase in agitation speed will result in a decrease in microsphere size, since higher agitation speeds will result in greater shear stress. />
Therefore, the SU-8 film can be used for preparing microspheres with small size and good uniformity, and the pressure intensity is closely related to the flow rate and the stirring speed of the discrete phase because the rupture of the film is caused by overlarge bearing pressure intensity, so that the flow rate of the discrete phase can be increased to 4500 mu l.h by using the film -1 (stirring speed was 100 rpm). Likewise, the agitation speed can be further increased from 100rpm, resulting in increased shear provided by the continuous phase and a further decrease in the size of the microspheres produced.
To sum up, the film that this patent provided can be under the great condition of discrete phase flow volume or stirring speed, produce the microballon that small-size, degree of consistency are better. This result is determined by the multilayer structure of the film (film thickness of 1 μm for a pore size of 1 μm is 1 μm, and film thickness of 20 μm for a pore size of 20 μm is 20 μm).
The present description sets forth the design, fabrication, and testing of a membrane emulsification device. The novel film is characterized by a multilayer structure, and the strength of the film is greatly improved while the small aperture can be ensured by the multilayer structure. The film is made of SU-8 series photoresist by adopting a photoetching technology. The test result shows that the microspheres prepared by the film have good performance in the aspects of size and uniformity. Since the SU-8 photoresist is low in price, the photolithography technology has become a rather mature microfluidic processing technology, and the film also has great advantages in terms of cost. To the authors' knowledge, this is also the first application of SU-8 photoresist to the fabrication of thin film emulsification devices.
The present application has been described in relation to the above embodiments, which are only examples for implementing the present application. It must be noted that the disclosed embodiments do not limit the scope of the application. Rather, modifications and equivalent arrangements included within the spirit and scope of the claims are included within the scope of the present application.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The above embodiments of the present application are described in detail, and specific examples are applied in the present application to explain the principles and implementations of the present application, and the description of the above embodiments is only used to help understand the technical solutions and core ideas of the present application; those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the present disclosure as defined by the appended claims.
Claims (7)
1. A thin film emulsification device for making discrete phase microspheres, comprising: a thin film having a plurality of via structures for passing the discrete phases;
the thin film comprises a first photoresist layer and a second photoresist layer, the through hole structure comprises a first through hole arranged on the first photoresist layer and a second through hole arranged on the second photoresist layer, and the second through hole is correspondingly communicated with the first through hole; the thickness of the first photoresist layer is smaller than that of the second photoresist layer, and the size of the first through hole is smaller than that of the second through hole;
the first through hole and the second through hole are both in a square shape, and are coaxially arranged in a direction vertical to the film;
the cross section of the first through hole and the cross section of the second through hole are both square, and the side of the first through hole and the side of the second through hole are arranged in parallel;
the thickness of the first photoresist layer is equal to the length of the side of the cross section of the first through hole, and the thickness of the second photoresist layer is equal to the length of the side of the cross section of the second through hole;
the membrane emulsification device also comprises a discrete phase feeding device which is connected with the second through hole side of the membrane and is used for controlling the flow of the discrete phase supplied to the membrane; wherein the thickness of the thin film is 21 μm, the thickness of the first photoresist layer is 1 μm, the length of the side of the cross section of the first through hole is 1 μm, the thickness of the second photoresist layer is 20 μm, and the length of the side of the cross section of the second through hole is 20 μm.
2. The membrane emulsification device of claim 1, further comprising:
a magnetic stirrer to provide shear to the discrete phases, wherein the direction of the shear is perpendicular to the direction of flow of the discrete phases.
3. The thin film emulsification device according to claim 2 wherein said magnetic stirrer is provided with a receptacle for holding the continuous phase and for receiving the manufactured discrete phase microspheres.
4. A method for manufacturing the thin film emulsification device according to claim 1 comprising the steps of forming a thin film;
the step of manufacturing the film comprises:
manufacturing a metal layer on a glass substrate, coating photoresist on the metal layer and carrying out patterning treatment to form a first photoresist layer, wherein a first through hole is formed in the first photoresist layer;
etching the metal layer and reserving the metal layer below the first photoresist layer;
coating photoresist on the glass substrate and the first photoresist layer and carrying out patterning treatment to form a second photoresist layer, wherein a second through hole is formed in the second photoresist layer and is correspondingly communicated with the first through hole; the size of the first through hole is smaller than that of the second through hole; and
and etching to remove the glass substrate and the residual metal layer.
5. The method of claim 4,
the step of coating photoresist on the metal layer and patterning to form a first photoresist layer comprises: arranging a first mask plate above the coated photoresist, wherein the first mask plate is provided with a first shading area and a first light transmitting area, the first light transmitting area is in the shape of the cross section of a first through hole, the photoresist corresponding to the first shading area is washed and removed by a developer after the photoresist is exposed, baked and cured by laser, and a first photoresist layer is formed after oxygen plasma cleaning; the step of coating photoresist on the glass substrate and the first photoresist layer and patterning to form a second photoresist layer comprises: set up the second mask plate in the photoresist top of coating, the second mask plate is equipped with second shading area and second printing opacity district, the shape in second printing opacity district is the cross section of second through-hole, through laser exposure and toast the solidification behind the photoresist will correspond the back is washed to the developer for the photoresist in second shading area and is got rid of, washes with isopropyl alcohol and carries out the drying with nitrogen gas after and form second photoresist layer.
6. The method of claim 4, wherein the metal layer comprises chromium, and the glass substrate is removed by hydrofluoric acid etching.
7. The method of claim 4, further comprising, prior to the etching to remove the glass substrate and remaining metal layer:
and sealing and attaching vent pipes of the discrete phase feeding devices on the second photoresist layer around the second through holes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210002531.9A CN114534647B (en) | 2022-01-04 | 2022-01-04 | Film emulsifying device and manufacturing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210002531.9A CN114534647B (en) | 2022-01-04 | 2022-01-04 | Film emulsifying device and manufacturing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114534647A CN114534647A (en) | 2022-05-27 |
| CN114534647B true CN114534647B (en) | 2023-04-18 |
Family
ID=81669577
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210002531.9A Active CN114534647B (en) | 2022-01-04 | 2022-01-04 | Film emulsifying device and manufacturing method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114534647B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003012957A (en) * | 2001-04-27 | 2003-01-15 | Canon Inc | Colored composition for color filter containing microcapsuled pigment comprising polyhydroxyalkanoate |
| CN106492715A (en) * | 2016-12-19 | 2017-03-15 | 广东工业大学 | A kind of method and device for preparing microgranule |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5651900A (en) * | 1994-03-07 | 1997-07-29 | The Regents Of The University Of California | Microfabricated particle filter |
| EP1908512A1 (en) * | 2002-07-15 | 2008-04-09 | Asahi Glass Company, Limited | Process for producing inorganic spheres |
| JP3723201B1 (en) * | 2004-10-18 | 2005-12-07 | 独立行政法人食品総合研究所 | Method for producing microsphere using metal substrate having through hole |
| WO2007136328A1 (en) * | 2006-05-18 | 2007-11-29 | Marilyn Rayner | Manufacturing method of a membrane and a membrane thereof, for emulsification |
| US20090023189A1 (en) * | 2007-05-18 | 2009-01-22 | Applera Corporation | Apparatus and methods for preparation of subtantially uniform emulsions containing a particle |
| CN101497067B (en) * | 2009-01-16 | 2011-11-09 | 北京航空航天大学 | Preparation method for assembling large-area ordered microsphere template by liquid level swirl method |
| CN102096326B (en) * | 2009-12-14 | 2012-12-05 | 中芯国际集成电路制造(上海)有限公司 | Double exposure method and etching method |
| CN102243435B (en) * | 2011-04-20 | 2012-08-22 | 合肥工业大学 | Method for preparing micro-nanometer fluid system through compound developing of positive and negative photoresists |
| JP6207007B2 (en) * | 2012-05-15 | 2017-10-04 | 国立大学法人 千葉大学 | Liposomes and production methods thereof |
| CN107298426B (en) * | 2016-04-14 | 2019-07-05 | 中国科学院苏州纳米技术与纳米仿生研究所 | Magnetic microchip, preparation method and application with encoding of graphs |
-
2022
- 2022-01-04 CN CN202210002531.9A patent/CN114534647B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003012957A (en) * | 2001-04-27 | 2003-01-15 | Canon Inc | Colored composition for color filter containing microcapsuled pigment comprising polyhydroxyalkanoate |
| CN106492715A (en) * | 2016-12-19 | 2017-03-15 | 广东工业大学 | A kind of method and device for preparing microgranule |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114534647A (en) | 2022-05-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Bhagat et al. | Photodefinable polydimethylsiloxane (PDMS) for rapid lab-on-a-chip prototyping | |
| Nan et al. | Engineered elastomer substrates for guided assembly of complex 3D mesostructures by spatially nonuniform compressive buckling | |
| US10391485B2 (en) | Microfluidic electrocage device and cell medium for trapping and rotating cells for live-cell computed tomography (CT) | |
| US9375873B2 (en) | Curved and flexible microfluidics | |
| CN102243435B (en) | Method for preparing micro-nanometer fluid system through compound developing of positive and negative photoresists | |
| CN106391151A (en) | Manufacturing method of multilayer microfluidic chip suitable for batch production | |
| CN101585508B (en) | Preparation method of organic glass micro-fluidic chip based on photosensitive thixotrope film | |
| CN114534647B (en) | Film emulsifying device and manufacturing method thereof | |
| CN111334403A (en) | Micro-bubble generation chip based on micro-fluidic and preparation method and application thereof | |
| CN110354925A (en) | It is a kind of comprising can deformation liquid metal electrode micro-fluidic chip and preparation method thereof | |
| Miller et al. | Lift-off of large-scale ultrathin nanomembranes | |
| US9030746B2 (en) | Fabrication method of microlens array and microlens array thereof | |
| CN114527525A (en) | Method for making artificial compound eye | |
| CN104627952B (en) | A kind of flexible super-hydrophobic superoleophobic structure preparation method | |
| CN100456063C (en) | Optical element, method of producing optical elements, coating device, and coating method | |
| Nam et al. | Generation of 3D microparticles in microchannels with non-rectangular cross sections | |
| Gao et al. | Direct optical micropatterning of poly (dimethylsiloxane) for microfluidic devices | |
| Xue et al. | Simplest method for creating micropatterned nanostructures on PDMS with UV Light | |
| CN107367836B (en) | Electrowetting device and preparation method thereof | |
| CN106744654B (en) | A kind of method for preparing transverse circular micro coaxle metal structure on a silicon substrate | |
| US20210023559A1 (en) | Microfluidic devices with tunable wettability and solvent resistance and methods for manufacturing the same | |
| CN109759154A (en) | A kind of micro-fluidic chip and preparation method thereof based on polypyrrole electrochemical transistor | |
| CN116214779A (en) | Microporous membrane forming and manufacturing method | |
| CN110862926A (en) | Multilayer paper chip based on microfluidic technology and construction method thereof | |
| CN101332650A (en) | Casting die for preparing elastic plastics casting with three dimensional structure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |