CN114536652A - Method for preparing microfluidic chip through injection molding of nickel composite electroforming mold core - Google Patents
Method for preparing microfluidic chip through injection molding of nickel composite electroforming mold core Download PDFInfo
- Publication number
- CN114536652A CN114536652A CN202210170978.7A CN202210170978A CN114536652A CN 114536652 A CN114536652 A CN 114536652A CN 202210170978 A CN202210170978 A CN 202210170978A CN 114536652 A CN114536652 A CN 114536652A
- Authority
- CN
- China
- Prior art keywords
- injection molding
- mold core
- microfluidic chip
- nickel composite
- electroforming
- 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.)
- Granted
Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 117
- 238000005323 electroforming Methods 0.000 title claims abstract description 94
- 239000002131 composite material Substances 0.000 title claims abstract description 82
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 59
- 238000001746 injection moulding Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000000463 material Substances 0.000 claims abstract description 42
- 239000000243 solution Substances 0.000 claims abstract description 29
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 25
- 239000010703 silicon Substances 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 23
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000010931 gold Substances 0.000 claims abstract description 16
- 229910052737 gold Inorganic materials 0.000 claims abstract description 16
- 239000003093 cationic surfactant Substances 0.000 claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 238000011049 filling Methods 0.000 claims abstract description 9
- 238000005507 spraying Methods 0.000 claims abstract description 9
- 238000003760 magnetic stirring Methods 0.000 claims abstract description 7
- 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
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 15
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000002245 particle Substances 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
- -1 Polytetrafluoroethylene Polymers 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 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
- 238000009826 distribution Methods 0.000 claims description 5
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 5
- 239000004793 Polystyrene Substances 0.000 claims description 4
- 239000012811 non-conductive material Substances 0.000 claims description 4
- 239000002861 polymer material Substances 0.000 claims description 4
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 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
- 238000005429 filling process Methods 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical group FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 description 10
- 238000003756 stirring Methods 0.000 description 7
- 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
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229920002120 photoresistant polymer Polymers 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 3
- 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
- 239000004327 boric acid Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000000465 moulding 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
- 229920006125 amorphous polymer Polymers 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000520 microinjection Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052961 molybdenite Inorganic materials 0.000 description 2
- 239000002090 nanochannel Substances 0.000 description 2
- 238000001259 photo etching Methods 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 group 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process 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
- 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
Images
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 female die and a composite electroforming solution; s2, carrying out vacuum coating and gold spraying conductive treatment on the silicon female die; s3, placing the silicon master die subjected to gold spraying and electric conduction treatment in the composite electroforming solution for core electroforming, and then cleaning and drying to obtain a nickel composite electroforming core; s4, performing injection molding filling, pressure maintaining, cooling and demolding processes on the nickel composite electroforming mold core, and bonding a substrate and a cover plate to obtain a microfluidic chip for chemical detection and analysis; the composite electroforming solution is obtained by dissolving a cationic surfactant in a pure nickel electroforming solution, adding a low-surface-energy material, and dispersing by magnetic stirring. The invention prepares the microfluidic chip by injection molding of the nickel composite electroforming mold core, and can realize high-quality, large-batch and low-cost manufacture.
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 of biochemical analysis, has the advantages of integration, high efficiency, convenience and the like, and the micro-nano channel structure of the chip is the key for realizing the function of the micro-nano channel structure, so that the realization of high-quality forming of the micro-fluidic chip channel structure is always a hot point of research. The common manufacturing methods of microfluidic chips include hot stamping, 3D printing and injection molding, wherein the injection molding has been the main mode of commercial mass production due to its advantages of low cost and short molding cycle.
The injection molding process comprises four parts of filling, pressure maintaining, cooling and demolding, the demolding process is used as a key part in injection molding manufacturing, and the existence of various factors can cause the defects of microstructure demolding adhesion, surface roughness, fracture, size deviation and the like, so that the service performance of the microstructure is influenced. When the structural dimension of the part is reduced to a micro/nano scale, the demolding resistance is mainly acted by the combination of adhesion and friction. The surface quality of the mold core is a key influencing the micro-structure forming quality of the micro-fluidic chip, and the surface modification treatment is widely used for improving the surface performance of the mold core, reducing the surface energy, the friction coefficient and the like and improving the demolding quality of injection molding.
The traditional surface coating treatment is used for modifying the mold core, so that the service life of the coating is short, and the requirement of injection molding mass production is difficult to meet. The existing polymer forming through a composite electroforming mold core is only used in the hot stamping process, the use environments of the mold core are different, and the application of the nickel composite electroforming mold core in the injection molding process of a microfluidic chip is not reported.
Therefore, it is necessary to provide a method for preparing a microfluidic chip by injection molding of a nickel composite electroforming 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, in which a low surface energy material is added to a pure nickel electroforming solution, and the low surface energy material and nickel ions are co-deposited under the action of a cationic surfactant to obtain the nickel composite electroforming mold core, so as to improve the surface performance of the mold core, and to implement high-quality and large-batch injection molding preparation of the microfluidic chip, the preparation method including the steps of:
s1, preparing a silicon female die and a composite electroforming solution;
s2, carrying out vacuum coating and gold spraying conductive treatment on the silicon female die;
s3, placing the silicon master die subjected to gold spraying and electric conduction treatment in the composite electroforming solution for core electroforming, and then cleaning and drying to obtain a nickel composite electroforming core;
s4, performing injection molding filling, pressure maintaining, cooling and demolding processes on the nickel composite electroforming mold core, and bonding a substrate and a cover plate to obtain a microfluidic chip for chemical detection and analysis;
the composite electroforming solution is obtained by dissolving a cationic surfactant in a pure nickel electroforming solution, adding a low-surface-energy material, and dispersing by magnetic stirring.
Furthermore, the micro-fluidic chip is of a micro-channel structure with the depth of 40-80 microns and the width of 40-200 microns, and the reaction gas used for etching is SF6Or C4F8。
Further, the thickness of the conductive gold layer in the vacuum coating gold 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) or molybdenum disulfide (MoS)2) Or tungsten disulfide (WS)2) The particle size/flake size distribution is 80-200 nm, and the particles are insoluble in deionized water.
Further, the cationic surfactant is a fluorocarbon compound, and the fluorocarbon compound is Cetyl Trimethyl Ammonium Bromide (CTAB) or perfluorooctyl quaternary ammonium iodide (FC-134).
Further, the nickel composite electroforming mold core in the 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 during the injection molding filling process in S4 is: the melt temperatures of the PC, the COC, the PMMA and the PS are respectively 280-300 ℃, 270-290 ℃, 260-280 ℃ and 270-290 ℃, and the filling rate is 20-45 cm3/s。
Further, in the S4, the bonding pressure of the substrate and the cover plate 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.
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 micro-fluidic 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 cationic surfactant and metal nickel ions in the electroforming solution are jointly deposited to form a composite mold core in the electroforming process;
the structure of the composite electroforming mold core is determined by the structural requirements of the microfluidic chip, and the structural design of the silicon master mold can be carried out according to the actual requirements, 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 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 silicon female die structure can be designed according to actual requirements, and the preparation of the nickel composite electroforming die core with different structures such as micro-columns and grooves is realized;
(2) the invention selects the nano material with low surface energy characteristic, can reduce the surface energy and the friction coefficient of the pure nickel mold core, improves the surface wear resistance of the mold core and prolongs the service life of the mold core;
(3) the invention adopts the injection molding method to prepare the polymer microfluidic chip, and can realize the manufacture with high quality, large batch and low cost.
Drawings
FIG. 1 is a process flow diagram of an embodiment of the invention;
FIG. 2 is a schematic diagram of an apparatus for manufacturing a nickel composite electroforming core according to an embodiment of the present invention;
fig. 3 is a structural diagram of a microfluidic chip prepared according to an embodiment of the present invention.
[ description of reference ]
1-a direct current power supply; 2-a cathode; 3-a silicon master mold; 4-nickel composite electroforming mold core; 5-low surface energy materials; 6-an active agent; 7-heating plate; 8-a cathode; 9-titanium basket; 10-pure nickel plate; 11-nickel ions; 12-a magnetic stirrer; 13-a liquid inlet; 14-a microchannel; 15-a liquid outlet; 16-a substrate; 17-cover slip.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
Unless defined otherwise, the terms 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, etc. used in the present invention may be commercially available or may be prepared by existing methods.
Aiming at the existing problems, 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 preparing a microfluidic chip by injection molding of a nickel composite electroforming mold core according to the present invention.
Fig. 2 is a schematic diagram of a device for preparing a nickel composite electroforming mold core in the method for preparing a microfluidic chip by injection molding of the nickel composite electroforming mold core according to the present invention.
Example 1
A method for preparing a microfluidic chip by injection molding of a nickel composite electroforming mold core comprises the following specific implementation flows:
s1: and finishing the preparation of the micro-fluidic chip silicon female die by adopting precision equipment such as an ultraviolet photoetching machine, an etching machine and the like. The micro-channel structure of the micro-fluidic chip has the depth of 60 mu m and the width of 120 mu m. Based on the 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 the silicon plate, and carrying out exposure treatment on the photoresist by using an ultraviolet photoetching machine through a mask plate after drying treatment; developing the exposed photoresist, etching the developed silicon plate by using a deep silicon etching machine, wherein the reaction gas used for etching is SF6(ii) a And finally, removing the photoresist on the surface of the etched silicon plate to obtain the silicon female die with the inverse structure of the microfluidic chip.
S2: and (2) carrying out gold spraying electric conduction treatment on the silicon master die in the step (1) by adopting a high vacuum coating instrument, and depositing a layer of gold film on the surface of the silicon master die to enable the surface of the silicon master die to become an electric conduction layer for mass transfer and deposition of cations in the electroforming solution. In order to ensure the dimensional accuracy of the microstructure, the thickness of the gold layer for the conductive treatment is 30nm, and the shape and the size of the surface structure are not influenced.
S3: and (3) placing the silicon female die sprayed with gold in the step (2) in composite electroforming solution dispersed with low surface energy materials to prepare the nickel composite electroforming mold core. First, 350g/L nickel sulfate (NiSO) was weighed using an electronic balance4) 40g/L nickel chloride (NiCl)2) 40g/L boric acid (H)3BO3) Adding intoAnd (3) fully dissolving the nickel in ionized water for more than 60min by using magnetic stirring to obtain a pure nickel electroforming solution, wherein the pH value of the solution is 3.2-3.5. And then adding 0.1g/L cationic surfactant, magnetically stirring for 45min, fully dissolving, adding 0.5g/L low-surface-energy material, and magnetically stirring and dispersing for more than 60min to obtain the uniformly dispersed composite electroforming solution.
In the step, the selected low surface energy material is Polytetrafluoroethylene (PTFE), the particle size distribution of the material is 80-200 nm, and the material does not have conductivity and is insoluble in deionized water.
In this step, cetyl trimethylammonium bromide (CTAB) is selected as the cationic surfactant to be added. 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 co-deposition with metal nickel ions in the electroforming solution in the electroforming process is realized to form the composite mold core.
In the step, a pure nickel plate is used as an anode and is placed in a metal titanium basket for supplementing metal nickel ions in the composite electroforming solution in the electroforming process, a silicon female die is used as a cathode, and two polar plates are symmetrically placed in an electroforming tank at a distance of 6 cm.
In the step, a direct current power supply is adopted in the composite electroforming process of the nickel mold core, and the current density is selected to be 3A/dm2The thickness of the core is determined by the electroforming time.
In the step, in order to prevent the low surface energy material from settling under the action of gravity and influencing the performance of the composite electroforming mold core, magnetic stirring is always used in the electroforming process, the rotating speed of the magnetic stirring is 600rpm, and the temperature of the composite electroforming liquid is 50 ℃ in the electroforming process.
In the step, the nickel composite electroforming mold core after electroforming is cleaned by absolute ethyl alcohol ultrasonic wave for 7min and deionized water ultrasonic wave for 7min, and the cleaned mold core is placed in a 50 ℃ oven for 4min for drying.
In the step, the obtained nickel composite electroforming mold core has better surface smoothness, and the low surface energy material PTFE is uniformly distributed. Because the addition amount of the low-surface-energy material PTFE 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 a mold in a mold thermal bonding injection molding mold, the mold is arranged on a German Arburg370S type precision injection molding machine, the filling, pressure maintaining, cooling and demolding processes of injection molding are completed, a micro-fluidic chip containing a micro-channel structure is obtained after the substrate and the cover plate are bonded, and the micro-fluidic chip 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 common material for microfluidic chips, and the amorphous polymer material is Polycarbonate (PC).
In this step, the melt temperature during filling of injection molding 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 30cm3And/s, the mold temperature is 120 ℃, the pressure maintaining pressure is 150MPa, and the pressure maintaining time is 7 s.
In the step, the substrate and the cover plate are aligned by opening the mold after pressure maintaining, the mold is closed again to complete the in-mold thermal bonding process of the substrate and the cover plate, 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, wherein the substrate comprises a micro-channel structure, and the cover plate is a flat plate without a structure.
In the step, the micro-channel structure of the micro-fluidic chip is successfully prepared by injection molding, the deformation defects such as structural fracture and the like do not occur, 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.
Preferably, the nickel composite electroforming mold core prepared in step S3 can be used in a hot stamping process to realize batch preparation of microfluidic chips.
More preferably, in step S4, the bonding process between the microfluidic chip substrate and the cover plate can be performed by using an out-of-mold bonding method, which can be selected from solvent bonding, ultrasonic bonding, etc.
Example 2
The difference from the embodiment 1 is that:
s3: the silicon female die sprayed with gold in the step (2) is placed in a position with dispersed lowAnd (3) preparing a nickel composite electroforming mold core in the composite electroforming solution of the surface energy material. First, 350g/L nickel sulfate (NiSO) was weighed using an electronic balance4) 40g/L nickel chloride (NiCl)2) 40g/L boric acid (H)3BO3) Adding into deionized water, and dissolving with magnetic stirring for more than 60min to obtain pure nickel electroforming solution with pH of 3.2-3.5. And then adding 0.1g/L cationic surfactant, magnetically stirring for 45min, fully dissolving, adding 5g/L low-surface-energy material, and magnetically stirring and dispersing for more than 60min to obtain the uniformly dispersed composite electroforming solution.
In the step, the selected low surface energy material is Polytetrafluoroethylene (PTFE), the particle size distribution of the material is 80-200 nm, and the material does not have conductivity 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 smoothness, and the low surface energy material PTFE is uniformly distributed. The surface smoothness of the composite mold core prepared in example 1 is slightly worse, because more PTFE is added to cause certain agglomeration, and PTFE with larger particle size is formed to be 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 demoulding 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 core, so that the surface energy of the core is reduced. The surface roughness of the microchannels is slightly greater due to the slightly less planar surface of the resulting composite core.
Example 3
The difference from the embodiment 1 is that:
s3: and (3) placing the silicon female die sprayed with gold in the step (2) in composite electroforming solution dispersed with low surface energy materials to prepare the nickel composite electroforming mold core. First, 350g/L nickel sulfate (NiSO) was weighed using an electronic balance4) 40g/L nickel chloride (NiCl)2) 40g/L boric acid (H)3BO3) Adding into deionized water, magnetically stirring to dissolve for more than 60min to obtain pure nickel electroforming solutionThe pH value of (A) is 3.2-3.5. And then adding 0.1g/L cationic surfactant, magnetically stirring for 45min, fully dissolving, adding 0.5g/L low-surface-energy material, and magnetically stirring and dispersing for more than 60min to obtain the uniformly dispersed composite electroforming solution.
In this step, the low surface energy material selected is molybdenum disulfide (MoS)2) The sheet diameter of the material is 80-200 nm, and the material itself has no conductivity 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 smoothness and low surface energy material MoS2The distribution is even. The surface smoothness of the composite mold core prepared in the embodiment 1 is better.
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. This is due to MoS2As an important solid lubricant, the self-lubricating composite mold core has a low friction coefficient, plays a role in reducing friction in the composite mold core and reduces the friction in the demolding process.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A method for preparing a microfluidic chip by injection molding of a nickel composite electroforming mold core is characterized by comprising the following steps:
s1, preparing a silicon female die and a composite electroforming solution;
s2, carrying out vacuum coating and gold spraying conductive treatment on the silicon female die;
s3, placing the silicon master die subjected to gold spraying and electric conduction treatment in the composite electroforming solution for core electroforming, and then cleaning and drying to obtain a nickel composite electroforming core;
s4, performing injection molding filling, pressure maintaining, cooling and demolding processes on the nickel composite electroforming mold core, and bonding a substrate and a cover plate to obtain a microfluidic chip for chemical detection and analysis;
the composite electroforming solution is obtained by dissolving a cationic surfactant in a pure nickel electroforming solution, adding a low-surface-energy material, and dispersing by magnetic stirring.
2. The method for preparing a microfluidic chip through injection molding of the nickel composite electroforming mold core according to claim 1, wherein the microfluidic chip is of a micro-channel structure with the depth of 40-80 μm and the width of 40-200 μm, and the reaction gas used for etching is SF6Or C4F8。
3. The method for preparing a microfluidic chip through 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 and gold 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 for preparing a microfluidic chip through nickel composite electroforming mold core injection molding according to claim 1, wherein 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) The particle size/flake size distribution is 80-200 nm, and the particles are insoluble in deionized water.
5. The method for preparing a microfluidic chip through injection molding of the nickel composite electroforming mold core according to claim 1, wherein the cationic surfactant is a fluorocarbon, and the fluorocarbon is Cetyl Trimethyl Ammonium Bromide (CTAB) or perfluorooctyl quaternary ammonium iodide (FC-134).
6. The method for preparing the microfluidic chip through the nickel composite electroforming core injection molding according to claim 1, wherein the nickel composite electroforming 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 ℃.
7. The method for preparing the microfluidic chip through nickel composite electroforming mold core injection molding according to claim 1, wherein the non-crystalline 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).
8. The method for preparing the microfluidic chip through the nickel composite electroforming mold core injection molding according to claim 7, wherein the melt temperature during the injection molding filling process in S4 is: the melt temperatures of the PC, the COC, the PMMA and the PS are respectively 280-300 ℃, 270-290 ℃, 260-280 ℃ and 270-290 ℃, and the filling rate is 20-45 cm3/s。
9. The method for preparing the microfluidic chip through the nickel composite electroforming mold core injection molding according to claim 1, wherein the bonding pressure of the substrate and the cover plate in 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210170978.7A CN114536652B (en) | 2022-02-23 | 2022-02-23 | Method for preparing micro-fluidic chip through injection molding of nickel composite electroforming mold core |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210170978.7A CN114536652B (en) | 2022-02-23 | 2022-02-23 | Method for preparing micro-fluidic chip through injection molding of nickel composite electroforming mold core |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114536652A true CN114536652A (en) | 2022-05-27 |
| CN114536652B CN114536652B (en) | 2024-05-10 |
Family
ID=81677542
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210170978.7A Active CN114536652B (en) | 2022-02-23 | 2022-02-23 | Method for preparing micro-fluidic chip through injection molding of nickel composite electroforming mold core |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114536652B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117261089A (en) * | 2023-11-22 | 2023-12-22 | 湘潭大学 | Manufacturing method of micro-fluidic chip based on dual-mode injection molding |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4534831A (en) * | 1982-09-27 | 1985-08-13 | Inoue-Japax Research Incorporated | Method of and apparatus for forming a 3D article |
| JPH11350182A (en) * | 1998-06-12 | 1999-12-21 | Ricoh Co Ltd | Production of optical disk stamper and electroforming liquid |
| DE19853445A1 (en) * | 1998-11-19 | 2000-05-25 | Siemens Ag | Contact pins, for semiconductor chip test cards, are produced by electroforming pin tips and adjoining spring stirrups using structured resist layers |
| JP2009167497A (en) * | 2008-01-18 | 2009-07-30 | Mepj:Kk | Electroformed product and electroforming method |
| CN101733884A (en) * | 2009-12-25 | 2010-06-16 | 温州大学 | Method for manufacturing micro gear |
| JP2012193395A (en) * | 2011-03-15 | 2012-10-11 | Kanagawa Prefecture | Ni-W ELECTROFORMING SOLUTION FOR MOLDING DIE, METHOD FOR PRODUCING MOLDING DIE, MOLDING DIE, AND METHOD FOR PRODUCING MOLDED ARTICLE |
| CN102788831A (en) * | 2012-08-13 | 2012-11-21 | 中国科学院研究生院 | Microfluidic chip electrophoretic-electrochemical detecting device with adjustable pH after separation and use thereof |
| CN102910574A (en) * | 2012-11-01 | 2013-02-06 | 北京工业大学 | Manufacturing method for non-silicon MEMS micro-channel group |
| CN108160124A (en) * | 2016-12-07 | 2018-06-15 | 中国科学院大连化学物理研究所 | Micro-fluidic chip with gradual change microchannel height, its preparation template and method |
| WO2018131960A1 (en) * | 2017-01-13 | 2018-07-19 | 성낙훈 | Mold fabricated by electroforming and method for fabricating same |
| CN111686831A (en) * | 2020-07-06 | 2020-09-22 | 中南大学 | Preparation method of micro-fluidic chip in-mold solvent bonding |
-
2022
- 2022-02-23 CN CN202210170978.7A patent/CN114536652B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4534831A (en) * | 1982-09-27 | 1985-08-13 | Inoue-Japax Research Incorporated | Method of and apparatus for forming a 3D article |
| JPH11350182A (en) * | 1998-06-12 | 1999-12-21 | Ricoh Co Ltd | Production of optical disk stamper and electroforming liquid |
| DE19853445A1 (en) * | 1998-11-19 | 2000-05-25 | Siemens Ag | Contact pins, for semiconductor chip test cards, are produced by electroforming pin tips and adjoining spring stirrups using structured resist layers |
| JP2009167497A (en) * | 2008-01-18 | 2009-07-30 | Mepj:Kk | Electroformed product and electroforming method |
| CN101733884A (en) * | 2009-12-25 | 2010-06-16 | 温州大学 | Method for manufacturing micro gear |
| JP2012193395A (en) * | 2011-03-15 | 2012-10-11 | Kanagawa Prefecture | Ni-W ELECTROFORMING SOLUTION FOR MOLDING DIE, METHOD FOR PRODUCING MOLDING DIE, MOLDING DIE, AND METHOD FOR PRODUCING MOLDED ARTICLE |
| CN102788831A (en) * | 2012-08-13 | 2012-11-21 | 中国科学院研究生院 | Microfluidic chip electrophoretic-electrochemical detecting device with adjustable pH after separation and use thereof |
| CN102910574A (en) * | 2012-11-01 | 2013-02-06 | 北京工业大学 | Manufacturing method for non-silicon MEMS micro-channel group |
| CN108160124A (en) * | 2016-12-07 | 2018-06-15 | 中国科学院大连化学物理研究所 | Micro-fluidic chip with gradual change microchannel height, its preparation template and method |
| WO2018131960A1 (en) * | 2017-01-13 | 2018-07-19 | 성낙훈 | Mold fabricated by electroforming and method for fabricating same |
| CN111686831A (en) * | 2020-07-06 | 2020-09-22 | 中南大学 | Preparation method of micro-fluidic chip in-mold solvent bonding |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117261089A (en) * | 2023-11-22 | 2023-12-22 | 湘潭大学 | Manufacturing method of micro-fluidic chip based on dual-mode injection molding |
| CN117261089B (en) * | 2023-11-22 | 2024-02-02 | 湘潭大学 | Manufacturing method of micro-fluidic chip based on dual-mode injection molding |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114536652B (en) | 2024-05-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100468846C (en) | Composite dual-electrode plates preparation method of minisize directly connecting methanol fuel battery | |
| CN101205054B (en) | Minitype metal nickel mould producing method | |
| CN100585491C (en) | Large area periodic array three-dimensional microstructure preparation method | |
| Zhang et al. | Investigation of mass transfer inside micro structures and its effect on replication accuracy in precision micro electroforming | |
| CN101051184B (en) | Large area micro nano structure soft impression method | |
| CN114536652B (en) | Method for preparing micro-fluidic chip through injection molding of nickel composite electroforming mold core | |
| CN1693182A (en) | Deep submicron three-dimensional rolling mould and its mfg. method | |
| CN112927862B (en) | High-performance large-area flexible transparent electrode and preparation method and application thereof | |
| CN101071871B (en) | Composite bipolar plate for miniature fuel cell and its preparing method | |
| CN108153108A (en) | A kind of large scale is without splicing micro-nano mould manufacturing method | |
| CN110350288A (en) | The efficient integral manufacturing method of the batch of Terahertz hollow rectangular waveguide | |
| Zhang et al. | Study of ion transportation and electrodeposition under hybrid agitation for electroforming of variable aspect ratios micro structures | |
| Guan et al. | Synthesis of two-dimensional WS2/nickel nanocomposites via electroforming for high-performance micro/nano mould tools | |
| CN108615892B (en) | Modified current collector for effectively inhibiting uncontrolled growth of dendritic crystal of lithium metal battery, and preparation method and application thereof | |
| Matsumura et al. | Fabrication of copper damascene patterns on polyimide using direct metallization on trench templates generated by imprint lithography | |
| KR102330451B1 (en) | A roll stamp for imprint apparatus and a manufacturing method of the same | |
| Zhao et al. | Fabrication of metal microfluidic chip mold with coplanar auxiliary cathode in the electroforming process | |
| CN102671730A (en) | Polymeric microfluidic chip integrating nickel column microarrays and preparation method thereof | |
| Zhao et al. | Experimental study on uniformity of copper layer with microstructure arrays by electroforming | |
| CN107394558B (en) | Impression block and the method that micro-structure is formed on the coating of conductive terminal | |
| Jochem et al. | Solution-based, additive fabrication of flush metal conductors in plastic substrates by printing and plating in two-level capillary channels | |
| CN108693700B (en) | Imprint template and preparation method thereof | |
| Schanz et al. | Microelectroforming of metals | |
| CN113290770A (en) | Injection molding method of plastic microfluidic chip | |
| TW448084B (en) | Manufacture method of microstructure with high aspect ratio |
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 |