CN113372502A - Solid-liquid current conversion device and method for materials in micropores - Google Patents

Solid-liquid current conversion device and method for materials in micropores Download PDF

Info

Publication number
CN113372502A
CN113372502A CN202110581806.4A CN202110581806A CN113372502A CN 113372502 A CN113372502 A CN 113372502A CN 202110581806 A CN202110581806 A CN 202110581806A CN 113372502 A CN113372502 A CN 113372502A
Authority
CN
China
Prior art keywords
solid
liquid
solution
current conversion
mold
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.)
Pending
Application number
CN202110581806.4A
Other languages
Chinese (zh)
Inventor
牛万灏
陈小明
王春江
王硕邦
邵金友
徐超凡
李祥明
陈小亮
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian Jiaotong University
Original Assignee
Xian Jiaotong University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Xian Jiaotong University filed Critical Xian Jiaotong University
Priority to CN202110581806.4A priority Critical patent/CN113372502A/en
Publication of CN113372502A publication Critical patent/CN113372502A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F271/00Macromolecular compounds obtained by polymerising monomers on to polymers of nitrogen-containing monomers as defined in group C08F26/00
    • C08F271/02Macromolecular compounds obtained by polymerising monomers on to polymers of nitrogen-containing monomers as defined in group C08F26/00 on to polymers of monomers containing heterocyclic nitrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y80/00Products made by additive manufacturing
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/46Polymerisation initiated by wave energy or particle radiation
    • C08F2/48Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light

Abstract

A solid-liquid current conversion device and method for materials in micropores are disclosed, (1) a two-dimensional photoetching microchannel mold, a three-dimensional structure soluble resin mold or a PDMS mold is prepared; (2) using a mould to complete the molding of the microporous structure; (3) qualitatively analyzing the surface properties of the two-dimensional and three-dimensional molds and the properties of the used dissolving solution, and carrying out interface and environment regulation, wherein the PDMS mold does not need to be regulated; (4) placing the mold in a forced convection device; (5) and starting the forced convection device, and stopping working when the concentration of the soluble material in the solution in the filtering chamber is reduced to a set threshold value, so as to complete solid-liquid current conversion in the micropores. A set of high-efficiency forced convection device is designed according to the regulation and control of solid-liquid interface properties and solid-liquid current conversion environment in the micropores, so that the problems that materials in the micropore structure are difficult to dissolve, the dissolving quality of a typical micro-nano processing structural member is limited by structural openness and a dissolving surface, the dissolving efficiency of soluble photosensitive resin in a three-dimensional micropore structure is low, the dissolving rate is slow and the like are solved.

Description

Solid-liquid current conversion device and method for materials in micropores
Technical Field
The invention is suitable for the fields of micro-nano manufacturing technology and micro-nano processing technology, particularly relates to a solid-liquid current conversion device and a method for a material in a micropore, and particularly provides a device capable of realizing forced solid-liquid current conversion for the material in the micropore through the processes of interface regulation, environment regulation and forced convection so as to realize high-efficiency and high-quality solid-liquid current conversion for the material in the micropore.
Background
In recent years, with the rapid development of micro-nano manufacturing processes, the forming method of micro-structured devices is gradually diversified, and technologies such as surface exposure stereo micro-lithography not only facilitate the structural design of micro-devices, but also further improve the forming precision of the structured devices. However, the requirements of the technology on materials and processing environment are too high, so that most of materials still cannot be subjected to high-precision structured molding, and the turnover molding process is greatly expanded and applied in the micro-scale direction.
The method has the advantages of obvious mold turnover forming advantages, greatly expanded material selection range, integrated forming, fewer defects of the manufactured component compared with a forward processing technology, greatly improved quality, high processing efficiency, good economy and the like. The mold turnover forming process applied to the field of micro-nano processing still has the problem under the traditional condition, for example, liquid materials can not be smoothly poured into a microporous mold under the action of air pressure in the pouring process. Therefore, in the aspect of turnover processing in the micro-nano field, micropore perfusion and micropore filling technologies are all important factors influencing processing quality. In the device turnover process, the pouring quality and the pouring efficiency of the material in the micropores directly determine whether the forming structure has defects or not and the forming cost. For example, if air or other impurities are mixed in during the pouring process, the formed structure is obviously shrunk or broken, and the forming quality is seriously influenced. Based on this, Wei He et al, the university of electronics, has studied via filling processes in the manufacture of high density interconnect printed circuit boards using multiple physical coupling techniques, via filling using SPS (bis (sodium-thiopropyl) -disulfide), EO/PO (ethylene oxide and propylene oxide block copolymer), and pepi (polyethylene oxide-polyimide), but its poor material selectivity is still an important factor that limits its further development. Clementine M et al, by stanford university, constructed a channel of the desired pattern in the PU matrix by photolithography and etching techniques, and embedded conductive carbon nanotubes to form electrodes, thereby producing a flexible electronic skin. However, the development of the flexible electronic skin is greatly influenced by the problems of high dissolving cost, low dissolving speed and the like of the PU matrix; yu Song et al, Beijing university, delivers PDMS composite material through a vacuum pump and permeates through capillary force, pours the PDMS composite material into a porous structure of a sugar cube, and dissolves the sugar cube in hot water to prepare porous PDMS sponge, but the problems of low pouring precision, slow dissolution rate and the like exist in the dissolution process of the sugar cube; in addition to the problem of dissolution of soluble materials in random three-dimensional structures, Kanguk Kim et al of California university use BTO and other materials to directly perform digital stereolithography to form three-dimensional structures, but because BTO absorbs ultraviolet light, the BTO-doped photosensitive material has low stereolithography precision and low efficiency, an inverse structure mold containing the BTO structure is selected to be formed, and a required structure is obtained by a mode of mold turning, but the problems that the structured soluble resin mold has small contact surface with a dissolving solution in a microporous cavity, the dissolving rate is low, complete dissolution is difficult and the like always restrict the development of the method. In summary, the current conversion method for solid-liquid materials in the microporous structure still has the defects and disadvantages of high dissolution cost, slow dissolution rate, incomplete dissolution, insufficient contact between the soluble materials and the dissolution solution, and the like, which causes the molding quality of the microporous structure to be difficult to ensure, and the cost to be expensive, and needs to be optimized and improved.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a device and a method for solid-liquid current conversion of materials in micropores, wherein a set of high-efficiency forced convection device is designed according to the regulation and control of the solid-liquid interface property and the solid-liquid current conversion environment in the micropores, so that the problems of difficulty in dissolving materials in a micropore structure, limitation of structural openness and a dissolving surface on the dissolving quality of a typical micro-nano processing structural member, low dissolving efficiency of soluble photosensitive resin in a three-dimensional micropore structure, slow dissolving rate and the like are solved, the quality of a microcolumn structure based on a mold-turning manufacturing method is improved, and the forming cost of the microcolumn structure is reduced.
In order to achieve the purpose, the invention provides a specific scheme as follows:
a solid-liquid current conversion device for materials in micropores comprises a shell 1, wherein a working chamber 2 is fixed on one side in the shell 1, three working spaces, namely an A working space 3, a B working space 5 and a C working space 7, are arranged in the working chamber 2 and are separated by a hollowed working space partition plate 6, and a fixing clamp 4 is arranged on the working space partition plate 6 as required; a filter chamber 11 communicated with the working chamber 2 is arranged above the other side in the shell 1, a water level sensor 10 is arranged in the filter chamber 11, and a filter paper layer 12 is arranged at the bottom of the filter chamber; a water pump 14 is arranged in the space below the filter chamber 11, and the water outlet of the water pump 14 is communicated with the water inlet of the working chamber 2.
The solid-liquid current conversion method based on the solid-liquid current conversion device for the materials in the micropores comprises the following steps:
(1) preparing a required two-dimensional photoetching micro-channel mold, a soluble resin mold with a three-dimensional structure or a PDMS mold by using a 3D printing technology and a stereolithography technology, and performing corresponding post-treatment;
(2) coating the die prepared in the step (1) with a liquid insoluble material to be formed, and finishing the forming of the microporous structure when the insoluble material is solidified;
(3) interface and environment regulation and control are carried out according to the surface properties of the soluble two-dimensional and three-dimensional molds, the properties of the predicted used dissolving solution and the interaction relationship, and the PDMS molds do not need to be regulated and controlled;
(4) placing the die with the interface and environment regulation and control completed in the step (3) in a converter device for clamping;
(5) and starting the converter, stopping working when the concentration of the soluble material in the solution in the filtering chamber is reduced to a set threshold value, and finishing solid-liquid conversion in the micropores.
The two-dimensional photoetching microchannel mold is a photoetching microchannel mold obtained by photoetching and developing commercial AZ4620 photoresist.
The material of the soluble resin mould with the three-dimensional structure is soluble photosensitive resin, and the material preparation comprises the following components in parts by weight: selecting 40-60 parts of comonomer N, N-dimethylacrylamide or acrylamide, 40-60 parts of methacrylic acid, methyl methacrylate or sodium acrylate and 40-50 parts of crosslinking cracking agent methacrylic anhydride or N, N-methylene bisacrylamide, heating the mixture in an oil bath at the temperature of 40-60 ℃, mixing the mixture, and then respectively adding 90-120 parts of filler and 10-20 parts of photoinitiator for uniform dispersion; the filler comprises polyvinyl alcohol, polyvinylpyrrolidone or methylcellulose; the photoinitiator comprises acylphosphine oxide or bis-benzoylphenylphosphine oxide.
The post-treatment is the removal of uncured resin in the soluble resin mold and the subsequent ultraviolet overexposure so as to achieve the complete curing molding of the designed resin mold.
The liquid insoluble material includes, but is not limited to, one of the following: paraffin, PDMS, silicone rubber and epoxy resin.
The dissolving solution includes but is not limited to one of the following: 1-5mol/L NaOH solution, 1-5mol/L KOH solution, 1-10mol/L HCL solution, 1-3mol/L H2SO4Solution, DMF or butylamine organic solvent.
The interface regulation and control is to regulate and control the concentration and viscosity of the selected dissolving solution and the properties of surface smoothness and hydrophilicity and hydrophobicity of the soluble material and balance the interaction relationship of the two; if the dissolving solution is an inorganic solution, the concentration of the dissolving solution needs to be adjusted according to the material of the microporous structure matrix, so that the contact angle of the dissolving solution is as small as possible, and the dissolving solution can more easily enter the microporous structure and is contacted with the soluble mold; if the dissolving solution is an organic solution, the organic solution with the contact angle as small as possible is selected according to the material of the microporous structure substrate, and the dissolving solution can easily enter the microporous structure and contact with the soluble mold.
The environment regulation and control is selected according to the optimal working environment of the selected dissolving solution, if the selected dissolving solution is a volatile solution, a high-pressure low-temperature environment is selected to reduce the volatilization of the dissolving solution and improve the utilization rate of the dissolving solution; if the solution is a high-melting organic solution, a relatively high-temperature environment should be selected to ensure sufficient fluidity.
The converter device arranged in the step (4) is specifically as follows: for a three-dimensional structure, fixing the structure in a vertical horizontal plane direction by using a working space division plate 6; for a two-dimensional structure, it is fixed using a fixing clip 4.
The step (5) is specifically as follows: supplying 5-12V direct current to a water pump 14, starting the whole cycle, forcing water flow to enter the bottom of a working chamber through the pressurization of the water pump, further flowing upwards under the action of water pressure, sequentially passing through three working spaces, forcing solid-liquid current conversion on a workpiece to be processed, when the water level exceeds a partition plate between the working chamber 2 and a filtering chamber 11, enabling current conversion waste liquid to enter the filtering chamber 11, filtering through filter paper 12, enabling the waste liquid to enter the water pump again, entering the next current conversion cycle, monitoring the water level in the filtering chamber 11 in real time by a water level sensor 10, automatically closing the water pump 14 when the water level exceeds a threshold value, and starting the water pump again when the water level drops to a safety value, so that the waste liquid is prevented from entering the next cycle without being processed.
The invention has the beneficial effects that:
(1) the method for interface regulation and environment regulation realizes the stable matching of properties of the solution, the soluble mould material and the indissolvable structural material, solves the problems of difficult solid-liquid contact, insufficient current conversion, damage to a microporous structure in the current conversion process and the like during solid-liquid current conversion in micropores, and provides reliable guarantee for subsequent forced solid-liquid current conversion.
(2) The forced current conversion method designed by the invention provides a high-quality and high-efficiency processing means for solid-liquid current conversion in the micropores on the basis of interface regulation and environment regulation, greatly improves the quality of micro-nano processing, ensures complete dissolution and removal of soluble substances in the pores compared with the traditional direct forming method, and provides a feasible scheme for preparing the microporous structure by die rollover.
(3) The forced convection device for providing power for solid-liquid conversion in the micropores is an implementation means of a forced convection method, is prepared by a 3D printing technology, and is simple in structure, easy to manufacture and low in cost; the forced solid-liquid current conversion can be simultaneously carried out on a plurality of two-dimensional or three-dimensional workpieces, the efficiency is high, and the compatibility is good; the filtering operation can ensure the full utilization of the dissolving solution, and the environment is friendly; the water level monitoring device monitors the filtering chamber in real time, and has high automation degree and high safety factor.
Drawings
FIG. 1 is a technical scheme diagram of a solid-liquid conversion method for materials in micropores provided by the invention.
Fig. 2 is a schematic view of the photocuring 3D printing of the soluble photosensitive resin according to the present invention.
FIG. 3 is a schematic view of a soluble resin mold provided by the present invention.
Fig. 4 is a schematic view of paraffin injection of the soluble resin mold provided by the present invention.
FIG. 5 is a schematic view of the interface regulation provided by the present invention.
FIG. 6 is a schematic diagram of the structure and internal operation of the device according to the present invention.
Fig. 7 is a schematic diagram of forced commutation within micropores in a forced convection apparatus provided by the present invention.
FIG. 8 is a schematic diagram of the preparation of sponge PDMS according to the present invention.
Fig. 9 is a schematic diagram of preparation of a two-dimensional channel-shaped plane and forced solid-liquid conversion provided by the present invention, wherein: 1 is photoresist or other light-cured material, and 2 is a liquid material of a structure to be formed.
FIG. 10 is a schematic view of a mounting clip for mounting a two-dimensional structure material according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to preferred examples thereof.
Referring to fig. 6, the solid-liquid converter for the materials in the micropores according to the present invention is applied to all the following embodiments, and includes a device housing 1, the device housing 1 is fixed with a working chamber 2 through a fixing jaw 8, the working chamber 2 includes three working spaces, which are respectively a working space a 3, a working space B5 and a working space C7, the three working spaces are separated by a hollow working space partition plate 6, and a fixing clip 4 is installed on the working space partition plate 6 according to requirements; a filter chamber 11 communicated with the working chamber 2 is arranged above the other side in the device shell 1, a water level sensor 10 is arranged in the filter chamber 11, and a filter paper layer 12 is arranged at the bottom of the filter chamber; a water pump 14 is arranged in the space below the filter chamber 11, and the water outlet of the water pump 14 is communicated with the water inlet of the working chamber 2.
Example 1
The embodiment is to realize the 3D printing and forming of the soluble resin mold and the solid-liquid conversion and dissolution in the paraffin micropores thereof, and referring to fig. 1, the specific process comprises the following steps:
(1) preparing a two-dimensional photoetching microchannel mould and a three-dimensional structure soluble resin mould by using a 3D printing technology and a stereolithography technology, and performing corresponding post-treatment;
preparation of a resin mold:
60g of comonomer N, N-dimethylacrylamide is weighed by an electronic scale and poured into a beaker for later use, then 60g of comonomer methyl methacrylate is weighed and poured into the beaker for mixing with the N, N-dimethylacrylamide, and then 45g of crosslinking cracking agent methacrylic anhydride is weighed and poured into the beaker for fully mixing the three. Putting the beaker containing the mixed solution into a magnetic stirring water bath kettle, and stirring for 30 minutes in an oil bath at 50 ℃; then, 120g of filler polyvinylpyrrolidone and 15g of photosensitizer aroylphosphine oxide are gradually added; continuously stirring for 3 hours at the temperature of 50 ℃ to obtain the soluble photosensitive resin. Referring to fig. 2, using the surface projection micro-stereolithography technique, a resin material 4 is placed in a resin tank 1, and every time a forming platform 3 is lowered by one layer thickness, an ultraviolet light emitter 2 exposes a corresponding shape of the layer, and the operation is repeated until the desired three-dimensional shape is completed. Referring to fig. 3, a resin mold is printed. And cleaning and drying the resin mold by deionized water for later use.
(2) And (3) coating the formed mould with a liquid insoluble material to be formed, and finishing the formation of the microporous structure after the insoluble material is solidified.
Weighing 100g of commercial solid paraffin by an electronic scale, placing the commercial solid paraffin in a small beaker, placing the beaker in a drying oven, setting the temperature at 100 ℃ for 1 hour, and obtaining the molten paraffin.
Preparing a paraffin microporous matrix: referring to fig. 4, the soluble resin mold prepared in the first step is placed in a small petri dish, taking care that the wall of the small petri dish is higher than the top of the resin mold. And injecting the molten liquid paraffin into the small culture dish at a higher temperature until the molten liquid paraffin overflows the top of the resin mold, slightly shaking the small culture dish to completely remove the air in the resin mold, and cooling the paraffin to obtain the paraffin microporous structure matrix of the soluble resin mold to be removed.
(3) And qualitatively analyzing the surface properties of the soluble two-dimensional and three-dimensional molds and the properties of the predicted used dissolving solution, and regulating and controlling the interface and the environment according to the respective properties and the interaction relationship.
The solution is a 1mol/L KOH solution, and the 1mol/L KOH solution is finally selected as the solution by an interface regulation method. The interface regulation schematic is shown in fig. 5.
56.1g KOH solids were weighed by electronic scale and placed in a beaker for use. 1L of deionized water is measured through a measuring cylinder, and the weighed KOH is slowly added into the deionized water while stirring until the KOH is completely dissolved. Cooling the solution to obtain 1mol/L KOH solution.
(4) And (4) placing the die which finishes interface and environment regulation and control in a forced current conversion device, clamping, and preparing for forced solid-liquid current conversion.
(5) And starting the converter, stopping working when the concentration of the soluble material in the solution in the filtering chamber is reduced to a set threshold value, and finishing solid-liquid conversion in the micropores.
Referring to fig. 6 and 7, the three-dimensional workpiece 9 to be processed, which is prepared in the second step, is fixed in any working space of the working chamber by the partition plate of the forced convection device, and then the working chamber, the filter chamber, the water pump and the like are all fixed in the device shell and the water level sensor is installed. And (4) slowly injecting the KOH dissolved solution prepared in the third step into the device along the inner edge of the filtering chamber until the water level is close to the water outlet of the working chamber. And finally, the water pump is communicated with 5-12v direct current to start the forced convection device. The dissolving solution is replaced once every 8 hours, and the current conversion is completed after 24 hours, thus obtaining the microporous paraffin matrix with the soluble resin completely dissolved.
Example 2
The embodiment is directed to a method for realizing solid-liquid conversion of a three-dimensional sponge structure by taking PDMS as a material, and with reference to FIG. 8, the method comprises the following steps:
(1) preparing a needed PDMS mold and carrying out corresponding post-treatment;
preparing a PDMS material:
60g polydimethysiloxane (PDMS, 184silicone elastomer base) is weighed by an electronic scale and poured into a beaker for standby, then 10g of curing agent is taken according to the mass fraction of 10:1, PDMS and the curing agent are mixed to obtain a matrix, a magnetic stirrer is placed into the mixture, the mixture is stirred for 10 minutes at the speed of 60rad/s by using a magnetic stirrer, and the mixture is placed into a vacuum pump after being fully stirred and is pumped to absolute vacuum to ensure that no bubbles exist in the PDMS.
(2) Coating the formed mould with a liquid insoluble material to be formed, and finishing the formation of the microporous structure after the insoluble material is solidified; the method specifically comprises the following steps:
2.1, preparing ball milling: the ball milling balls and the ball milling pot are flushed with ethanol and blown dry in a nitrogen environment. Weighing 50g of edible cube sugar by an electronic scale, adding the edible cube sugar into the cleaned ball milling tank, adding about 30 ball milling balls, covering the ball milling tank, and putting the ball milling tank into a ball milling instrument to mill for half an hour to obtain cube sugar particles with the size of 200 um.
2.2 mixing of cube sugar and PDMS.
And (3) completely adding the cubic sugar particles prepared in the second step into the PDMS prepared in the first step, and continuing stirring for 30min at a speed of 60rad/s by using a magnetic stirrer so as to uniformly disperse the cubic sugar in the PDMS. Putting the mixture of PDMS and the cubic sugar into an oven, and standing for 3h at the temperature of 80 ℃;
(3) the PDMS mold does not require regulation.
(4) And (4) placing the die which finishes interface and environment regulation and control in a current conversion device, clamping, and preparing to force solid-liquid current conversion.
(5) And starting the converter, stopping working when the concentration of the soluble material in the solution in the filtering chamber is reduced to a set threshold value, and finishing solid-liquid conversion in the micropores.
And cutting the solidified sample prepared in the third step into a required shape, placing the cut sample into a forced convection device, carrying out solid-liquid conversion according to the embodiment mode, replacing the aqueous solution once every 8 hours, and continuously dissolving for 24 hours to obtain the PDMS sponge structure with the microporous structure.
Example 3
The embodiment is to realize the high-efficiency solid-liquid conversion of a two-dimensional channel-shaped surface, and referring to fig. 9, the specific preparation process comprises the following steps:
(1) and preparing a required two-dimensional photoetching micro-channel mold, a soluble resin mold with a three-dimensional structure or a PDMS mold by using a 3D printing technology and a stereolithography technology, and performing corresponding post-treatment.
Preparing a photoetching microchannel mold:
selecting a PC plate (or a silicon wafer) as a photoresist substrate, carrying out ultrasonic treatment on the PC plate in alcohol for 10s, then placing the PC plate in a drying oven for drying at the set temperature of not higher than 60 ℃, and then coating photoresist AZ4620 on the PC plate by a spin coater at a low spin speed of 600 and at a high spin speed of 900, wherein the thickness of the photoresist is 15-17 mu m. And (3) placing the spin-coated photoresist on a 95 ℃ baking table for drying, then photoetching for 35s through a photoetching machine, and finally developing for 90s by using 0.5% sodium hydroxide as a developing solution. And (5) washing off the developing solution after the whole process is finished, and airing to obtain the photoresist mould.
(2) And (3) coating the formed mould with a liquid insoluble material to be formed, and finishing the formation of the microporous structure after the insoluble material is solidified.
Preparing a paraffin microchannel substrate, weighing 100g of commercial solid paraffin by an electronic scale, placing the paraffin in a small beaker, placing the beaker in an oven, setting the temperature at 100 ℃ for 1 hour, and obtaining the molten paraffin. And pouring molten paraffin onto the photoresist mould, slightly shaking the photoresist mould to fully fill the photoresist mould with the liquid paraffin, and cooling the paraffin to obtain the paraffin microchannel substrate connected with the photoresist mould.
(3) And qualitatively analyzing the surface properties of the soluble two-dimensional and three-dimensional molds and the properties of the predicted used dissolving solution, and regulating and controlling the interface and the environment according to the respective properties and the interaction relationship.
After analyzing the properties of paraffin and photoresist, alcohol which can dissolve the photoresist and does not react with the paraffin is selected as a dissolving solution.
(4) And (4) placing the die which finishes interface and environment regulation and control in a current conversion device, clamping, and preparing to force solid-liquid current conversion.
(5) And starting the converter, stopping working when the concentration of the soluble material in the solution in the filtering chamber is reduced to a set threshold value, and finishing solid-liquid conversion in the micropores.
Referring to fig. 10, the two-dimensional workpiece 15 to be processed obtained in the third step is fixed in any working space of the working chamber by the fixing clamp of the forced convection apparatus according to the present invention, and the working chamber, the filter chamber, the water pump, etc. are all fixed in the apparatus housing and the water level sensor is installed. And slowly injecting the selected alcohol into the device along the inner edge of the filtering chamber until the water level is close to the water outlet of the working chamber. And finally, the water pump is communicated with 5-12v direct current to start the forced convection device. The dissolving solution is replaced once every 8 hours, and the conversion is completed after 24 hours, so that the microchannel paraffin base body with the photoresist completely dissolved can be obtained. The whole solid-liquid forced current conversion dissolution work is completed.
The present invention includes but is not limited to the embodiments described above, and any equivalent or partial modifications made under the spirit of the present invention are considered to be within the scope of the present invention.

Claims (10)

1. A solid-liquid converter for materials in micropores comprises a device shell (1) and is characterized in that the device shell (1) is fixedly provided with a working chamber (2) through a fixing clamping jaw (8), the inside of the working chamber (2) comprises three working spaces which are respectively an A working space (3), a B working space (5) and a C working space (7), the three working spaces are separated through a hollowed working space partition plate (6), and a fixing clamp (4) is installed on the working space partition plate (6) according to requirements; a filter chamber (11) communicated with the working chamber (2) is arranged above the other side in the device shell (1), a water level sensor (10) is arranged in the filter chamber (11), and a filter paper layer (12) is arranged at the bottom of the filter chamber; a water pump (14) is arranged in the space below the filter chamber (11), and the water outlet of the water pump (14) is communicated with the water inlet of the working chamber (2).
2. The solid-liquid current conversion method of the solid-liquid current conversion device for the materials in the micropores is characterized by comprising the following steps:
(1) preparing a required two-dimensional photoetching micro-channel mold, a soluble resin mold with a three-dimensional structure or a PDMS mold by using a 3D printing technology and a stereolithography technology, and performing corresponding post-treatment;
(2) coating the formed mould with a liquid insoluble material to be formed, and finishing the formation of the microporous structure after the insoluble material is solidified;
(3) interface and environment regulation and control are carried out according to the surface properties of the soluble two-dimensional and three-dimensional molds, the properties of the predicted used dissolving solution and the interaction relationship, and the PDMS molds do not need to be regulated and controlled;
(4) placing the die which finishes interface and environment regulation in a current conversion device, clamping, and preparing to force solid-liquid current conversion;
(5) and starting the converter, stopping working when the concentration of the soluble material in the solution in the filtering chamber is reduced to a set threshold value, and finishing solid-liquid conversion in the micropores.
3. The method for solid-liquid conversion of a material inside a micro-pore according to claim 2,
the two-dimensional photoetching microchannel mold is a photoetching microchannel mold obtained by photoetching and developing commercial AZ4620 photoresist;
the soluble resin mould of three-dimensional structure be soluble photosensitive resin, its material preparation includes, according to weight fraction: selecting 40-60 parts of comonomer N, N-dimethylacrylamide or acrylamide, 40-60 parts of methacrylic acid, methyl methacrylate or sodium acrylate, and 40-50 parts of crosslinking cracking agent methacrylic anhydride or N, N-methylene bisacrylamide, mixing under heating of an oil bath at 40-60 ℃, then respectively adding 90-120 parts of filler and 10-20 parts of photoinitiator, and uniformly dispersing; the filler comprises polyvinyl alcohol, polyvinylpyrrolidone or methylcellulose; the photoinitiator comprises acylphosphine oxide or bis-benzoylphenylphosphine oxide.
4. The solid-liquid flow conversion method for materials in micropores according to claim 2, characterized in that the post-treatment is the removal of uncured resin inside the soluble resin mold and the subsequent ultraviolet overexposure to achieve the complete curing molding of the designed resin mold.
5. The method for solid-liquid conversion of a material inside a micro-pore according to claim 2, characterized in that said liquid insoluble material includes but is not limited to one of the following: paraffin, PDMS, silicone rubber and epoxy resin.
6. The method for solid-liquid conversion of materials in micropores according to claim 2, wherein the dissolving solution includes but is not limited to one of the following: 1-5mol/L NaOH solution, 1-5mol/L KOH solution, 1-10mol/L HCL solution, 1-3mol/L H2SO4 solution, DMF or butylamine organic solvent.
7. The method for solid-liquid current conversion of materials in micropores according to claim 2, wherein the interface regulation is to regulate the concentration and viscosity of the selected dissolving solution, and the properties of surface smoothness and hydrophilicity and hydrophobicity of the soluble materials, and balance the interaction relationship between the two; if the dissolving solution is an inorganic solution, the concentration of the dissolving solution needs to be adjusted according to the material of the microporous structure matrix, so that the contact angle of the dissolving solution is as small as possible, and the dissolving solution can more easily enter the microporous structure and is contacted with the soluble mold; if the dissolving solution is an organic solution, the organic solution with the contact angle as small as possible is selected according to the material of the microporous structure substrate, and the dissolving solution can easily enter the microporous structure and contact with the soluble mold.
8. The solid-liquid current conversion method for materials in micropores according to claim 2, wherein the environmental regulation is selected for the optimal working environment of the selected solution, and if the selected solution is a volatile solution, a high-pressure and low-temperature environment is selected to reduce the volatilization and improve the utilization rate of the solution; if the solution is a high-melting organic solution, a relatively high-temperature environment should be selected to ensure sufficient fluidity.
9. The solid-liquid current converting method for materials in micropores according to claim 2, wherein the current converting device placed in step (4) is specifically: aiming at a three-dimensional structure, fixing the three-dimensional structure in a vertical horizontal plane direction by using a working space division plate (6); for a two-dimensional structure, it is fixed using a fixing clip (4).
10. The method for solid-liquid conversion of a material in a micropore according to claim 2, wherein the step (5) is specifically: supplying 5-12V direct current to a water pump (14), starting the whole circulation, forcing water flow to enter the bottom of a working chamber through the pressurization of the water pump, further enabling the water flow to flow upwards under the action of water pressure and sequentially pass through three working spaces, forcing solid-liquid current conversion on a workpiece to be processed, when the water level exceeds a partition plate between the working chamber (2) and a filter chamber (11), enabling current conversion waste liquid to enter the filter chamber (11), enabling the current conversion waste liquid to enter the water pump again through the filtration of filter paper (12), enabling the current conversion waste liquid to enter the next current conversion circulation, monitoring the water level in the filter chamber (11) in real time by a water level sensor (10), automatically closing the water pump (14) when the water level exceeds a threshold value, and starting the current conversion waste liquid again when the water level drops to a safety value, so that the waste liquid is prevented from entering the next circulation without being processed.
CN202110581806.4A 2021-05-24 2021-05-24 Solid-liquid current conversion device and method for materials in micropores Pending CN113372502A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110581806.4A CN113372502A (en) 2021-05-24 2021-05-24 Solid-liquid current conversion device and method for materials in micropores

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110581806.4A CN113372502A (en) 2021-05-24 2021-05-24 Solid-liquid current conversion device and method for materials in micropores

Publications (1)

Publication Number Publication Date
CN113372502A true CN113372502A (en) 2021-09-10

Family

ID=77572370

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110581806.4A Pending CN113372502A (en) 2021-05-24 2021-05-24 Solid-liquid current conversion device and method for materials in micropores

Country Status (1)

Country Link
CN (1) CN113372502A (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110186081A1 (en) * 2010-01-05 2011-08-04 Stratasys, Inc. Support cleaning system
US20170036249A1 (en) * 2015-08-06 2017-02-09 David Jonathan Tofoya Removal of soluble support material with flow control

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110186081A1 (en) * 2010-01-05 2011-08-04 Stratasys, Inc. Support cleaning system
US20170036249A1 (en) * 2015-08-06 2017-02-09 David Jonathan Tofoya Removal of soluble support material with flow control

Similar Documents

Publication Publication Date Title
CN107176588B (en) A kind of preparation method of hollow microchannel structure
CN107500736A (en) A kind of ceramic paste for Stereolithography and preparation method thereof
CN106064261B (en) The System and method for of micro-pit array Electrolyzed Processing based on magnetic PDMS masks
CN103231518A (en) Polydimethylsiloxane array micropore film preparation method
CN107914333A (en) The method that zirconia ceramics cell phone rear cover is made using gel injection molding and forming technology
CN101717068B (en) Method for preparing polymeric micro-fluidic chip based on hydrogel male mold
CN113372502A (en) Solid-liquid current conversion device and method for materials in micropores
CN109759157B (en) Micro-fluidic chip for micro-bubble separation
CN108355727A (en) A kind of preparation method of micro-fluidic chip template
CN108000684A (en) A kind of adhesive for powder injection forming preparation method and applications
CN102799066B (en) Method for preparing concave lens array structure on titanium dioxide inorganic-organic photosensitive composite film
CN104708800A (en) Soft imprinting method for manufacturing micro-nano structure in cycloalkene polymer micro-fluidic chip
CN108031497A (en) A kind of micro-fluidic chip template and preparation method and application
CN116214779A (en) Microporous membrane forming and manufacturing method
CN109732920A (en) The 3D printing device and Method of printing of dusty material photocuring bonding
CN110039783B (en) Air filter for 3D biological printer and filtering method
CN105047525B (en) A kind of manufacture method of high-aspect-ratio flexible nano post array
CN1789108A (en) Secondary template duplicating process method based on dimethyl silicone polymer mini component
CN113977871A (en) Method for manufacturing bipolar plate
CN113211720A (en) Injection mold for PDMS micro-fluidic chip and manufacturing method
CN114434709B (en) Quick manufacturing method of concave micro-well and micro-channel
CN117244599B (en) Method for manufacturing PDMS micro-fluidic chip
CN206912174U (en) Multilayer Film automatic adhesive mechanism
CN117550547A (en) High-infiltration PDMS (polydimethylsiloxane) micropore array and manufacturing method thereof
CN101382742B (en) Developing method for mask plate

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
CB03 Change of inventor or designer information
CB03 Change of inventor or designer information

Inventor after: Chen Xiaoming

Inventor after: Wang Chunjiang

Inventor after: Xu Chaofan

Inventor after: Niu Wanhao

Inventor after: Wang Shuobang

Inventor after: Shao Jinyou

Inventor after: Li Xiangming

Inventor after: Chen Xiaoliang

Inventor before: Niu Wanhao

Inventor before: Chen Xiaoming

Inventor before: Wang Chunjiang

Inventor before: Wang Shuobang

Inventor before: Shao Jinyou

Inventor before: Xu Chaofan

Inventor before: Li Xiangming

Inventor before: Chen Xiaoliang

RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20210910