CN114536652B - Method for preparing micro-fluidic chip through injection molding of nickel composite electroforming mold core - Google Patents
Method for preparing micro-fluidic chip through injection molding of nickel composite electroforming mold core Download PDFInfo
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- CN114536652B CN114536652B CN202210170978.7A CN202210170978A CN114536652B CN 114536652 B CN114536652 B CN 114536652B CN 202210170978 A CN202210170978 A CN 202210170978A CN 114536652 B CN114536652 B CN 114536652B
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- nickel composite
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 238000005323 electroforming Methods 0.000 title claims abstract description 86
- 239000002131 composite material Substances 0.000 title claims abstract description 82
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 56
- 238000001746 injection moulding Methods 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 41
- 239000000243 solution Substances 0.000 claims abstract description 33
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 30
- 239000010703 silicon Substances 0.000 claims abstract description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 14
- 238000005507 spraying Methods 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 238000011049 filling Methods 0.000 claims abstract description 9
- 238000001771 vacuum deposition Methods 0.000 claims abstract description 6
- 238000004458 analytical method Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000001514 detection method Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 230000008569 process Effects 0.000 claims description 23
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000005530 etching Methods 0.000 claims description 8
- 229920002120 photoresistant polymer Polymers 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- 229920000089 Cyclic olefin copolymer Polymers 0.000 claims description 6
- 239000004713 Cyclic olefin copolymer Substances 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 6
- 239000004417 polycarbonate Substances 0.000 claims description 6
- 229920000515 polycarbonate Polymers 0.000 claims description 6
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000004793 Polystyrene Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 239000012811 non-conductive material Substances 0.000 claims description 4
- 239000002861 polymer material Substances 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920006125 amorphous polymer Polymers 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 3
- 238000001259 photo etching Methods 0.000 claims description 3
- 239000012495 reaction gas Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229940107816 ammonium iodide Drugs 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 description 10
- 229910001453 nickel ion Inorganic materials 0.000 description 6
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 238000000151 deposition Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 241000080590 Niso Species 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005429 filling process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000000520 microinjection Methods 0.000 description 2
- 239000002090 nanochannel Substances 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012742 biochemical analysis Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000002301 combined effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004049 embossing Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D1/00—Electroforming
- C25D1/10—Moulds; Masks; Masterforms
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/14—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor incorporating preformed parts or layers, e.g. injection moulding around inserts or for coating articles
- B29C2045/1486—Details, accessories and auxiliary operations
- B29C2045/14868—Pretreatment of the insert, e.g. etching, cleaning
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Moulds For Moulding Plastics Or The Like (AREA)
Abstract
The invention provides a method for preparing a microfluidic chip by injection molding of a nickel composite electroforming mold core, which comprises the following steps: s1, preparing a silicon master model and a composite electroforming solution; s2, carrying out vacuum coating, metal spraying and conductivity treatment on the silicon master model; s3, placing the silicon master model subjected to the metal spraying conductive treatment in the composite electroforming solution for electroforming of a mould core, and then cleaning and drying to obtain a nickel composite electroforming mould core; s4, carrying out injection molding filling, pressure maintaining, cooling and demolding on the nickel composite electroforming mold core, and bonding the substrate and the cover plate to obtain a microfluidic chip for chemical detection and analysis; the composite electroforming solution is obtained by dissolving a cationic surfactant in pure nickel electroforming solution, adding a low-surface-energy material, and dispersing by magnetic stirring. The micro-fluidic chip prepared by the injection molding of the nickel composite electroforming mold core can be manufactured in a large scale with high quality and low cost.
Description
Technical Field
The invention relates to the technical field of micro-injection molding and electroforming, in particular to a method for preparing a micro-fluidic chip through injection molding of a nickel composite electroforming mold core.
Background
The micro-fluidic chip is used as an important carrier for biochemical analysis, has the advantages of integration, high efficiency, convenience and the like, and the micro-nano channel structure of the chip is key for realizing the functions of the micro-nano channel structure, so that the realization of high-quality molding of the channel structure of the micro-fluidic chip is always a research hot spot. The commonly used manufacturing method of the microfluidic chip comprises hot stamping, 3D printing and injection molding technology, wherein the injection molding technology has the advantages of low cost and short molding period, and becomes a main mode of commercial mass production.
The injection molding process comprises four parts of filling, pressure maintaining, cooling and demolding, wherein the demolding process is used as a key part in injection molding manufacture, and the existence of various factors can cause defects such as microstructure demolding adhesion, surface roughness, fracture, size deviation and the like, so that the usability of the microstructure is affected. As part structural dimensions shrink to the micro/nano scale, the mold release resistance is primarily due to the combined effects of adhesion and friction. The surface quality of the mold core is the key for influencing the microstructure forming quality of the microfluidic chip, and the surface modification treatment is widely used for improving the surface performance of the mold core, reducing the surface energy and friction coefficient and the like, and is used for improving the injection molding demoulding quality.
The traditional surface coating treatment is used for carrying out mold core modification treatment, so that the service life of the coating is low, and the requirement of injection molding mass production is difficult to meet. The existing polymer molding process by the composite electroforming mold core is only used in the hot stamping process, the mold cores are different in use environment, and no report has been made on the injection molding process of the microfluidic chip by the nickel composite electroforming mold core.
Therefore, it is necessary to provide a method for preparing a microfluidic chip by injection molding of a nickel composite electroformed mold core.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for preparing a microfluidic chip by injection molding of a nickel composite electroforming mold core.
In order to achieve the above object, an embodiment of the present invention provides a method for preparing a microfluidic chip by injection molding of a nickel composite electroforming mold core, by adding a low surface energy material into a pure nickel electroforming solution, and co-depositing the low surface energy material and nickel ions under the action of a cationic surfactant to obtain the nickel composite electroforming mold core, improving the surface performance of the mold core, for realizing high-quality, mass injection molding preparation of the microfluidic chip, the preparation method comprising the steps of:
s1, preparing a silicon master model and a composite electroforming solution;
s2, carrying out vacuum coating, metal spraying and conductivity treatment on the silicon master model;
s3, placing the silicon master model subjected to the metal spraying conductive treatment in the composite electroforming solution for electroforming of a mould core, and then cleaning and drying to obtain a nickel composite electroforming mould core;
s4, carrying out injection molding filling, pressure maintaining, cooling and demolding on the nickel composite electroforming mold core, and bonding the substrate and the cover plate to obtain a microfluidic chip for chemical detection and analysis;
The composite electroforming solution is obtained by dissolving a cationic surfactant in pure nickel electroforming solution, adding a low-surface-energy material, and dispersing by magnetic stirring.
Furthermore, the micro-fluidic chip has a micro-channel structure with the depth of 40-80 mu m and the width of 40-200 mu m, and the reaction gas used for etching is SF 6 or C 4F8.
Further, the thickness of the conductive gold layer in the vacuum coating metal spraying conductive treatment is 10-50 nm, and the cleaning process is ultrasonic cleaning by using absolute ethyl alcohol and deionized water.
Further, the low surface energy material is a non-conductive material, and the low surface energy material is Polytetrafluoroethylene (PTFE), graphene Oxide (GO), molybdenum disulfide (MoS 2) or tungsten disulfide (WS 2), and the particle size/sheet diameter distribution is 80-200 nm and is insoluble in deionized water.
Further, the cationic surfactant is a fluorocarbon compound which is cetyl trimethylammonium bromide (CTAB) or perfluorooctyl quaternary ammonium iodide (FC-134).
Further, the nickel composite electroforming mold core in the step S4 is fixed on a mold, the mold is installed on an injection molding machine, and the temperature of the mold is 120 ℃.
Further, the amorphous polymer material used in the injection molding in S4 is one or more of Polycarbonate (PC), cyclic Olefin Copolymer (COC), polymethyl methacrylate (PMMA), and Polystyrene (PS).
Further, the melt temperature in the injection molding and filling process in S4: the melt temperatures of PC, COC, PMMA and PS are 280-300 ℃, 270-290 ℃, 260-280 ℃ and 270-290 ℃ respectively, and the filling rate is 20-45 cm 3/s.
Further, the bonding pressure between the substrate and the cover plate in the step S4 is 150-180 MPa, the bonding time is 150-300S, the demolding temperature is 75-85 ℃, the pressure maintaining pressure is 120-180 MPa, and the pressure maintaining time is 5-10S.
According to the invention, the low-surface-energy material is added into the pure nickel electroforming solution, and under the action of the cationic surfactant, the low-surface-energy material and nickel ions are jointly deposited to obtain the nickel composite electroforming mold core, so that the high-quality and large-batch injection molding preparation of the microfluidic chip is realized; the composite electroforming preparation of the injection molding mold core is carried out by adding the low surface energy material, so that the surface performance of the mold core is improved, the interaction between the polymer and the mold core in the injection molding process is reduced, and the injection molding quality of the micro-channel structure of the microfluidic chip is improved;
The low surface energy material dispersed in the composite electroforming solution is a non-conductive material, and the material has lower surface energy; the added cationic surfactant is adsorbed on the surface of the non-conductive low-surface-energy material, so that the added cationic surfactant and metal nickel ions in the electroforming solution are co-deposited to form a composite mold core in the electroforming process;
the structure of the composite electroforming mold core is determined by the structure requirement of the microfluidic chip, and the structure design of the silicon master mold can be carried out according to the actual requirement, so that the preparation of nickel composite electroforming mold cores with different structures is realized; the mold core prepared by composite electroforming realizes high-quality and batch production of the polymer microfluidic chip by adopting a micro injection molding mode; the mold core structure prepared by the composite electroforming can meet the use requirements of temperature and pressure in the injection molding process, and can be used for realizing batch preparation of microfluidic chips in the hot stamping process.
The scheme of the invention has the following beneficial effects:
(1) According to the scheme, the structure design of the silicon master model can be carried out according to actual requirements, and the preparation of nickel composite electroforming mold cores with different structures such as microcolumns, grooves and the like is realized;
(2) The nano material has low surface energy characteristic, so that the surface energy and friction coefficient of the pure nickel mold core can be reduced, the surface wear resistance of the mold core is improved, and the service life of the mold core is prolonged;
(3) The polymer micro-fluidic chip is prepared by adopting an injection molding method, and can be manufactured in a large scale with high quality and low cost.
Drawings
FIG. 1 is a process flow diagram of an embodiment of the present invention;
FIG. 2 is a schematic diagram of a manufacturing apparatus for a nickel composite electroformed mold core according to an embodiment of the invention;
Fig. 3 is a block diagram of a microfluidic chip fabricated according to an embodiment of the present invention.
[ Reference numerals description ]
1-A direct current power supply; 2-cathode; 3-silicon master; 4-nickel composite electroforming mold core; 5-a low surface energy material; 6-an active agent; 7-heating plate; 8-cathode; 9-titanium basket; 10-pure nickel plate; 11-nickel ions; 12-a magnetic stirrer; 13-a liquid inlet; 14-microchannel; 15-a liquid outlet; 16-a substrate; 17-cover plate.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved more apparent, the following detailed description will be given with reference to the accompanying drawings and specific embodiments.
Unless defined otherwise, the terms of art used in the present invention have the same meaning as commonly understood by one of ordinary skill in the art. The various raw materials, reagents, instruments, equipment and the like used in the present invention can be purchased commercially or prepared by existing methods.
The invention provides a method for preparing a microfluidic chip by injection molding of a nickel composite electroforming mold core.
Fig. 1 is a process flow diagram of a method for manufacturing a microfluidic chip by injection molding of a nickel composite electroformed mold core according to the present invention.
Fig. 2 is a schematic diagram of a device for manufacturing a microfluidic chip by injection molding of a nickel composite electroforming mold core according to the present invention.
Example 1
The method for preparing the micro-fluidic chip by the injection molding of the nickel composite electroforming mold core comprises the following specific implementation processes:
S1: and adopting a UV photoetching machine, an etching machine and other precise equipment to finish the preparation of the silicon master model of the microfluidic chip. The depth of the micro-channel structure of the micro-fluidic chip is 60 μm, and the width is 120 μm. Based on LIGA technology, a film material is utilized to process a micro-fluidic chip structure mask plate; coating a layer of positive photoresist on the surface of a silicon plate, and exposing the photoresist through a mask plate by using an ultraviolet photoetching machine after baking treatment; developing the exposed photoresist, and etching the developed silicon plate by using a deep silicon etching machine, wherein the reaction gas used for etching is SF 6; and finally, removing the photoresist on the surface of the etched silicon plate to obtain the silicon master model with the micro-fluidic chip reverse structure.
S2: and (3) carrying out metal spraying and conductivity treatment on the silicon master model in the step (1) by adopting a high vacuum coating instrument, and depositing a layer of metal film on the surface of the silicon master model to enable the surface of the silicon master model to be a conductive layer for cation mass transfer and deposition in electroforming solution. In order to ensure the dimensional accuracy of the microstructure, the thickness of the gold layer used for the conductive treatment is 30nm, and the shape and the size of the surface structure are not affected.
S3: and (3) placing the silicon master model subjected to metal spraying in the step (2) in composite electroforming solution in which a low-surface-energy material is dispersed to prepare the nickel composite electroforming mold core. Firstly, using an electronic balance to weigh 350g/L nickel sulfate (NiSO 4), 40g/L nickel chloride (NiCl 2) and 40g/L boric acid (H 3BO3) to be added into deionized water, and using magnetic stirring to fully dissolve for more than 60min to obtain pure nickel electroforming solution, wherein the pH value of the solution is 3.2-3.5. Then adding 0.1g/L cationic surfactant, magnetically stirring for 45min, fully dissolving, adding 0.5g/L low surface energy material, magnetically stirring and dispersing for more than 60min to obtain uniformly dispersed composite electroforming solution.
In this step, the selected low surface energy material is Polytetrafluoroethylene (PTFE), the particle size distribution of the material is 80-200 nm, the material itself is not conductive and is insoluble in deionized water.
In this step, the cationic surfactant added was chosen to be cetyltrimethylammonium bromide (CTAB). The cationic surfactant is adsorbed on the surface of the non-conductive material, so that the non-conductive low-surface-energy material has conductivity, and the composite mold core is formed by co-deposition with metal nickel ions in the electroforming solution in the electroforming process.
In the step, a pure nickel plate is used as an anode in the electroforming process, is placed in a metal titanium basket and is used for supplementing metal nickel ions in the composite electroforming solution in the electroforming process, a silicon master model is used as a cathode, and two polar plates are symmetrically placed in an electroforming tank, wherein the distance between the polar plates is 6cm.
In the step, the nickel mold core composite electroforming process adopts a direct current power supply, the current density is 3A/dm 2, and the mold core thickness is determined by the electroforming time.
In this step, in order to prevent the low surface energy material from settling under the action of gravity and affecting the performance of the composite electroforming mold core, magnetic stirring is always used in the electroforming process, the rotation speed of the magnetic stirring is 600rpm, and the temperature of the composite electroforming solution in the electroforming process is 50 ℃.
In the step, the nickel composite electroforming mold core after electroforming is cleaned by absolute ethyl alcohol in an ultrasonic manner for 7min, deionized water in an ultrasonic manner for 7min, and the cleaned mold core is placed in a 50 ℃ oven for 4min and dried.
In the step, the obtained nickel composite electroforming mold core has good surface finish, and the PTFE material with low surface energy is uniformly distributed. Because the PTFE addition amount of the low-surface-energy material is less, the PTFE content in the composite mold core is less.
S4: the nickel composite electroforming mold core in the step (3) is arranged on an in-mold thermal bonding injection molding mold, the mold is arranged on an Arburg370S type precise injection molding machine in Germany, filling, pressure maintaining, cooling and demolding processes of injection molding are completed, a micro-fluidic chip with a micro-channel structure is obtained after a substrate and a cover plate are bonded, and the micro-fluidic chip capable of being used for chemical detection and analysis is obtained after the substrate and the cover plate are bonded.
In this step, the polymer material used in the injection molding process is selected from the materials commonly used for microfluidic chips, and the amorphous polymer material is Polycarbonate (PC).
In this step, the melt temperature during the injection molding filling process was set according to the glass transition temperature of the material, the melt temperature of the material PC was set to 290℃and the filling rate was 30cm 3/s, the mold temperature 120℃and the dwell pressure was 150MPa, and the dwell time was 7s.
In the step, after pressure maintaining, the die is opened to align the substrate and the cover plate, and the die is closed again to finish the in-die bonding process of the substrate and the cover plate, wherein the bonding pressure in the bonding process is 160MPa, the bonding time is 220s, and the demolding temperature is 80 ℃. Finally, the micro-fluidic chip for chemical detection and analysis is obtained, as shown in fig. 3, the substrate contains a micro-channel structure, and the cover plate is a non-structural flat plate.
In the step, the micro-channel structure of the micro-fluidic chip is successfully prepared by injection molding, deformation defects such as structural fracture and the like are avoided, and the surface flatness of the channel structure is good. There is still some dimensional deviation due to errors in the composite core preparation and injection molding process.
More preferably, the nickel composite electroforming mold core prepared in the step S3 can be used for realizing batch preparation of microfluidic chips in a hot embossing process.
More preferably, in step S4, the bonding process of the microfluidic chip substrate and the cover sheet may be performed using an out-mold bonding method, and the bonding method may also be solvent bonding, ultrasonic bonding, or the like.
Example 2
The difference from example 1 is that:
S3: and (3) placing the silicon master model subjected to metal spraying in the step (2) in composite electroforming solution in which a low-surface-energy material is dispersed to prepare the nickel composite electroforming mold core. Firstly, using an electronic balance to weigh 350g/L nickel sulfate (NiSO 4), 40g/L nickel chloride (NiCl 2) and 40g/L boric acid (H 3BO3) to be added into deionized water, and using a magnetic stirring component to dissolve for more than 60min to obtain a pure nickel electroforming solution, wherein the pH value of the solution is 3.2-3.5. Then adding 0.1g/L cationic surfactant, magnetically stirring for 45min, fully dissolving, adding 5g/L low surface energy material, magnetically stirring and dispersing for more than 60min to obtain uniformly dispersed composite electroforming solution.
In this step, the selected low surface energy material is Polytetrafluoroethylene (PTFE), the particle size distribution of the material is 80-200 nm, the material itself is not conductive and is insoluble in deionized water.
The other steps are the same as in example 1.
The obtained nickel composite electroforming mold core has good surface finish, and PTFE which is a low surface energy material is uniformly distributed. Compared with the composite mold core prepared in the embodiment 1, the surface flatness of the composite mold core is slightly poorer, and the composite mold core has a certain agglomeration caused by more PTFE addition, so that PTFE with larger particle size is co-deposited in the composite mold core.
Compared with the micro-channel structure formed in the embodiment 1, the micro-fluidic chip has better forming quality, smaller deformation of the channel structure and lower demolding adhesion effect on the surface of the channel. This is due to the fact that more of the low surface energy material PTFE is co-deposited in the composite mould core, so that the surface energy of the mould core is reduced. The surface roughness of the micro-channels is slightly larger, which is caused by slightly poorer surface flatness of the obtained composite mold core.
Example 3
The difference from example 1 is that:
S3: and (3) placing the silicon master model subjected to metal spraying in the step (2) in composite electroforming solution in which a low-surface-energy material is dispersed to prepare the nickel composite electroforming mold core. Firstly, using an electronic balance to weigh 350g/L nickel sulfate (NiSO 4), 40g/L nickel chloride (NiCl 2) and 40g/L boric acid (H 3BO3) to be added into deionized water, and using a magnetic stirring component to dissolve for more than 60min to obtain a pure nickel electroforming solution, wherein the pH value of the solution is 3.2-3.5. Then adding 0.1g/L cationic surfactant, magnetically stirring for 45min, fully dissolving, adding 0.5g/L low surface energy material, magnetically stirring and dispersing for more than 60min to obtain uniformly dispersed composite electroforming solution.
In the step, the selected low-surface-energy material is molybdenum disulfide (MoS 2), the sheet diameter distribution of the material is 80-200 nm, and the material is not conductive and is insoluble in deionized water.
The other steps are the same as in example 1.
The obtained nickel composite electroforming mold core has good surface finish, and the low surface energy material MoS 2 is uniformly distributed. The surface smoothness of the composite mold core prepared in the embodiment 1 is better than that of the composite mold core prepared in the embodiment.
Compared with the micro-channel structure formed in the embodiment 1, the micro-fluidic chip has better forming quality, smaller deformation of the channel structure and smaller surface roughness of the micro-channel structure. The MoS 2 is used as an important solid lubricant, has a low friction coefficient, plays a role in antifriction in the composite mold core, and reduces the friction in the demolding process.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (8)
1. A method for preparing a microfluidic chip by injection molding of a nickel composite electroforming mold core, which is characterized by comprising the following steps:
s1, preparing a silicon master model and a composite electroforming solution;
s2, carrying out vacuum coating, metal spraying and conductivity treatment on the silicon master model;
s3, placing the silicon master model subjected to the metal spraying conductive treatment in the composite electroforming solution for electroforming of a mould core, and then cleaning and drying to obtain a nickel composite electroforming mould core;
s4, carrying out injection molding filling, pressure maintaining, cooling and demolding on the nickel composite electroforming mold core, and bonding the substrate and the cover plate to obtain a microfluidic chip for chemical detection and analysis;
The composite electroforming solution is obtained by dissolving a cationic surfactant in pure nickel electroforming solution, adding a low-surface-energy material, and magnetically stirring and dispersing; the low surface energy material is a non-conductive material, polytetrafluoroethylene (PTFE), graphene Oxide (GO), molybdenum disulfide (MoS 2) or tungsten disulfide (WS 2), and the particle size/sheet diameter distribution is 80-200 nm and is insoluble in deionized water;
Coating a layer of positive photoresist on the surface of a silicon plate, and exposing the photoresist through a mask plate by using an ultraviolet photoetching machine after baking treatment; developing the exposed photoresist, and etching the developed silicon plate by using a deep silicon etching machine; and finally, removing the photoresist on the surface of the etched silicon plate to obtain the silicon master model with the micro-fluidic chip reverse structure.
2. The method for preparing the micro-fluidic chip by the injection molding of the nickel composite electroforming mold core according to claim 1, wherein the micro-fluidic chip is of a micro-channel structure with the depth of 40-80 mu m and the width of 40-200 mu m, and the reaction gas used for etching is SF 6 or C 4F8.
3. The method for preparing the microfluidic chip by the injection molding of the nickel composite electroforming mold core according to claim 1, wherein the thickness of the conductive gold layer in the vacuum coating metal spraying conductive treatment is 10-50 nm, and the cleaning process is ultrasonic cleaning by using absolute ethyl alcohol and deionized water.
4. The method of manufacturing a microfluidic chip by nickel composite electroforming mold core injection molding according to claim 1, wherein the cationic surfactant is a fluorocarbon compound, which is cetyl trimethylammonium bromide (CTAB) or perfluorooctyl quaternary ammonium iodide (FC-134).
5. The method for manufacturing a microfluidic chip by injection molding of a nickel composite electroformed mold core according to claim 1, wherein the nickel composite electroformed mold core in S4 is fixed on a mold, the mold is mounted on an injection molding machine, and the mold temperature is 120 ℃.
6. The method for manufacturing a microfluidic chip by injection molding of a nickel composite electroformed mold core according to claim 1, wherein the amorphous polymer material used for injection molding in S4 is one or more of Polycarbonate (PC), cyclic Olefin Copolymer (COC), polymethyl methacrylate (PMMA), and Polystyrene (PS).
7. The method for manufacturing a microfluidic chip by injection molding of a nickel composite electroformed mold core according to claim 6, wherein the melt temperature during injection molding filling in S4: the melt temperatures of PC, COC, PMMA and PS are 280-300 ℃, 270-290 ℃, 260-280 ℃ and 270-290 ℃ respectively, and the filling rate is 20-45 cm 3/s.
8. The method for preparing the microfluidic chip by the injection molding of the nickel composite electroforming mold core according to claim 1, wherein the bonding pressure of the substrate and the cover plate in the step S4 is 150-180 MPa, the bonding time is 150-300S, the demolding temperature is 75-85 ℃, the holding pressure is 120-180 MPa, and the holding time is 5-10S.
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