CN104091620A - Method for manufacturing fusion pellet based on microfluid - Google Patents

Method for manufacturing fusion pellet based on microfluid Download PDF

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Publication number
CN104091620A
CN104091620A CN201410342972.9A CN201410342972A CN104091620A CN 104091620 A CN104091620 A CN 104091620A CN 201410342972 A CN201410342972 A CN 201410342972A CN 104091620 A CN104091620 A CN 104091620A
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Prior art keywords
microemulsion
phase
preparation
fusion
solution
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Inventor
顾忠泽
赵祥伟
谢卓颖
赵远锦
朱纪军
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Southeast University
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Southeast University
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00Energy generation of nuclear origin
    • Y02E30/10Nuclear fusion reactors

Abstract

The invention relates to a method for manufacturing a fusion pellet based on a microfluid channel, in particular to a method for manufacturing an inertial confinement nuclear fusion pellet based on a microfluid channel technology. According to the method, dual microemulsion is formed by pellet solutions or a front fusion body in a flowing phase by adopting a microfluid channel network system, the inner diameter and the outer diameter of the dual microemulsion are adjusted in real time through an image collecting and analysis system and a flow control system, and finally a preset size is achieved. Then, hollow micro balls meeting the ICF target requirements are formed through curing and drying based on a liquid drop formwork. According to the manufacturing method, the hollow micro balls which are uniform in size and controllable in ball wall can be manufactured, and the ICF requirements are met. The manufacturing method particularly comprises the first step of manufacturing the microfluid channel, the second step of manufacturing the microemulsion, the third step of obtaining the size of the microemulsion, the fourth step of controlling the inner diameter and the outer diameter of the dual emulsion and the fifth step of manufacturing the fusion pellet.

Description

Target capsule of fusion preparation method based on microfluid
Technical field
That the present invention relates to is a kind of preparation method of the inertial confinement fusion pellet based on microfluidic channel technology, belongs to technical field prepared by target capsule of fusion.
Background technology
Outstanding day by day along with energy problem, inertial confinement fusion (Inertial Confinement Fusion, ICF), as controllable nuclear fusion technology, receives increasing concern.The state such as American-European-Japanese is all being studied inertial confinement fusion.As the carrier of nuclear fusion fuel, development and the exploitation with the fusion target of tiny balloon structure are the important contents in ICF research.The preparation technology of pellet mainly contains at present: drop stove technology, xerogel technology, micro-packaging technology, interfacial polymerization etc.These methods need the instrument that precision is very high conventionally, and often consumption of raw materials is large, complex operation.Microflow control technique refers to employing Micrometer-Nanometer Processing Technology, on the chip of more than square centimeters, produce microchannel network structure, laboratory main equipment is integrated on as far as possible little operating platform, in order to complete different experimentations, and the technology that can analyze product.It not only makes the consumption of reagent reduce, and speed of experiment is improved, and expense reduces, and has fully demonstrated the development trend of microminiaturized, the integrated and portability of current laboratory equipment.Therefore, the pellet preparation method of exploitation based on microflow control technique will simplify experimental procedure, dwindle experimental facilities, accurately control result, realize a large amount of preparations of pellet.The present invention proposes a kind of new method of utilizing robotization microfluidic system to prepare inertial confinement fusion pellet.
Summary of the invention
Technical matters: the object of this invention is to provide a kind of target capsule of fusion preparation method based on microfluid.This preparation method makes the solution of pellet material or front aggressiveness form dual microemulsion by microfluidic channel, and according to the internal-and external diameter of the double emulsion calculating, regulate in real time the flow of each syringe pump to realize the control of double emulsion internal-and external diameter by imaging system, graphical analysis and control system, obtain the dual microemulsion of required size, dry by solidifying again, form the tiny balloon that meets the requirement of ICF target.This preparation method can prepare big or small homogeneous, and the tiny balloon that cyst wall is controlled meets the requirement of ICF target.
Technical scheme: the present invention is a kind of target capsule of fusion preparation method based on microfluid, this preparation method based on emulsion automatic creation system comprise the chip that generates microemulsion, the syringe pump that fluid flow is controlled, the imaging system of microemulsion size observation, graphical analysis and flow control system: adopt microfluidic channel network to make pellet solution or front aggressiveness in mobile phase, form dual microemulsion, the pattern of double emulsion sends control system to by imaging system and carries out the internal-and external diameter that graphical analysis obtains double emulsion, then by flow control system, regulate the flow of each syringe pump to realize the control of double emulsion internal-and external diameter, thereby realize the diameter of hollow pellet, wall thickness is controlled, its concrete preparation method comprises the following steps:
1) preparation of microfluidic channel: adopt micro-processing technology to set up microfluidic channel network system on silicon chip, glass, polymethylmethacrylate or dimethyl silicone polymer micro-fluid chip, this system has 3 entrances, be respectively capsule heart phase entrance, cyst wall phase entrance, mobile phase entrance, have 1 outlet;
2) preparation of microemulsion: capsule heart phase, cyst wall phase, mobile phase three-phase solution are respectively charged into three containers, are connected respectively 3 described entrances, control three-phase solution flow rate with digital control syringe pump, obtain uniform and stable microemulsion from outlet;
3) obtaining of microemulsion size: observe the generation situation of microemulsion by imaging system, the image of Real-time Collection microemulsion, goes out external diameter and the internal diameter of double emulsion by image analysis calculation;
4) control of double emulsion internal-and external diameter: the relation according between the internal-and external diameter value of the microemulsion calculating and they and three-phase solution flow rate, regulates three-phase solution flow rate automatically until the internal-and external diameter of microemulsion reaches the size precomputing;
5) preparation of target capsule of fusion: by microemulsion cyst wall dry solidification, remove capsule heart phase, obtain satisfactory hollow target capsule of fusion.
Microfluidic channel network system is 2 grades of T-shaped channel patterns, or converges shearing channel pattern.
By microemulsion imaging and analytic system and flow control system, realize the automatic control of double emulsion internal-and external diameter, thereby it is controlled to realize diameter, the wall thickness of hollow pellet.
Beneficial effect: according to the present invention, utilize micro-fluid chip to prepare target capsule of fusion and have the following advantages:
1) controllability is strong: because the design of microfluidic channel is fixed, only need regulator solution rate of flow of fluid can regulate and control diameter and the wall thickness of pellet.
2) liquid requirement is little: because microchannel is micron order or millimetre-sized, therefore can realize the flow velocity of μ l/min, reduce the waste of liquid.
3) preparation cost is low: a micro-fluid chip can be realized the preparation of sizes pellet, and the specification that only need change micro-fluid chip can realize the preparation of a series of pellets.
4) automaticity is high: the inside/outside diameter size system that only needs setting need to generate microemulsion just can regulate three-phase flow fast-growing to become required microemulsion automatically, gets final product diameter and the wall thickness of auto-control pellet.
Accompanying drawing explanation
Fig. 1 is 2 grades of T-shaped microfluidic channel schematic diagram of the present invention, and figure acceptance of the bid is marked with: capsule heart phase entrance 11, parietal layer phase entrance 12, mobile phase entrance 13, outlet 14, the first node 15, the second nodes 16.
Fig. 2 is that the present invention converges shearing microfluidic channel schematic diagram, and figure acceptance of the bid is marked with: capsule heart phase entrance 21, parietal layer phase entrance 22, mobile phase entrance 23, outlet 24, convergent point 25.
Fig. 3 is the embodiment of the present invention one schematic diagram, and figure acceptance of the bid is marked with: capsule heart phase entrance 31, parietal layer phase entrance 32, mobile phase entrance 33, outlet 34, the first node 35, the second nodes 36.
Fig. 4 is the schematic diagram of emulsion automatic creation system of the present invention, and figure acceptance of the bid is marked with: capsule heart phase entrance 37, and parietal layer phase entrance 38, mobile phase entrance 39, the first node 40, the second nodes 41, observe out 42, camera lens 43.
Embodiment
The present invention makes the solution of pellet material or the dual microemulsion of single dispersion that front aggressiveness forms specific dimensions automatically by robotization microfluidic system, drier by solidifying, and forms the tiny balloon that meets the requirement of ICF target.
Microfluidic channel network system of the present invention, this system can be 2 grades of T-shaped channel patterns, can be also to converge shearing channel pattern.Adopt micro-processing technology to set up microfluidic channel network system (comprising silicon, glass, polymethylmethacrylate, dimethyl silicone polymer micro-fluid chip) or select medical needle, polymer pipe (as Teflon, Peek, Polyvinylchloride), threeway (as Peek, stainless steel) etc. to connect a network channel system, this system has 3 entrances, be respectively capsule heart phase entrance, cyst wall phase entrance, mobile phase entrance, have 1 outlet.This microfluidic channel network, by effects such as the shearing force between water and oil phase, surface tension, has finally formed monodispersed W/O/W or the dual microemulsion of Water-In-Oil bag oil.
By imaging system, observe the generation situation of microemulsion, the image of Real-time Collection microemulsion, goes out external diameter and the internal diameter of double emulsion by image analysis calculation.According to the relation between the internal-and external diameter value of the microemulsion calculating and they and three-phase solution flow rate, automatically regulate three-phase solution flow rate until the internal-and external diameter of microemulsion reaches the size requiring in advance.
Collect the microemulsion of outlet, through dry solidification, form microcapsules, after the removal capsule heart, just formed hollow target capsule of fusion.
Microfluidic channel network system is 2 grades of T-shaped channel patterns, or converges shearing channel pattern.
Passage of the present invention has two kinds of method for makings: the one, and adopt micro-processing technology to set up microfluidic channel network system (comprising silicon, glass, polymethylmethacrylate, dimethyl silicone polymer micro-fluid chip); The 2nd, select medical needle, polymer pipe (as Teflon, Peek, Polyvinylchloride), threeway (as Peek, stainless steel) etc. to connect a network channel system.
Embodiment mono-: the preparation method of the polystyrene target capsule of fusion of diameter 500 μ m wall thickness 15 μ m
1. the preparation of passage:
1.. a length, be that 15cm internal diameter is to stamp an aperture on the Teflon tube wall of 500 μ m, insert No. 6 medical needles that polish in advance, attention will be inserted in syringe needle the centre of pipe, and this syringe needle is as the entrance of capsule heart solution (water);
2. No. 6 syringe needles are inserted in one end of .Teflon pipe, as the entrance of capsule wall solution (polystyrene solution);
3.. with the Peek threeway of internal diameter 500 μ m, connect the other end of this Teflon pipe and the Teflon pipe of the long 500 μ m internal diameters of other two 15cm, and insert No. 6 syringe needles in one end of a central Teflon pipe, as the entrance of mobile phase (polyvinyl alcohol water solution).
2. the preparation of microemulsion:
1.. 3.5g polystyrene (PS) is dissolved in to 25ml benzene and 25ml1, in the mixed solution of 2-ethylene dichloride, forms 7%PS solution;
2. .25g polyvinyl alcohol (PVA) (PVA) is dissolved in the middle of 500ml ultrapure water, forms 5%PVA solution;
3.. by water, PS solution, PVA solution is respectively charged into syringe, is loaded on digital control syringe pump, and the syringe of three-phase connects respectively capsule heart solution entrance, capsule wall solution entrance and mobile phase entrance;
4.. at software interface, setting pellet material is polystyrene; Solvent is benzene and 1,2-ethylene dichloride (1:1); Concentration is 7%; Required pellet diameter is 500 μ m, wall thickness 15 μ m.System is set three-phase flow velocity according to prevalue: the flow velocity of water is 0.5ml/h, and the flow velocity of PS solution is 1.5ml/h, and the flow velocity of PVA solution is 10ml/h.Then start emulsion generation system, when the first water (water) is when first node place and oil phase (PS solution) meet, form monodispersed water-in-oil emulsion; While meeting by second node and the second water (PVA solution) again, formed again monodispersed water-in-oil-in-water compositions.
5.. control system gathers the image of microemulsion and calculates external diameter and the internal diameter of double emulsion, according to the relation between the internal-and external diameter value of the microemulsion calculating and they and three-phase solution flow rate, automatically regulate three-phase solution flow rate until the internal-and external diameter of microemulsion reaches the size requiring in advance.When the microemulsion of outlet is stablized, with the 500ml round-bottomed flask that 250mlPVA solution is housed, receive.
3. the preparation of target capsule of fusion
1.. after receiving the microemulsion of some, round-bottomed flask is placed in to Rotary Evaporators, set temperature is 60 ℃, and rotating speed is 40rpm, starts rotation;
2.. when microemulsion is dry, emerge, temperature is made as to 70 ℃, rotating speed is adjusted to 60rpm;
3.. at the bottom of microemulsion sinks to bottle again, temperature is made as to 80 ℃, rotating speed is adjusted to 80rpm, maintains 1h;
4.. the solvent for the treatment of PS solution evaporates completely, takes out microballoon, cleans and removes surperficial PVA solution, and 60 ℃ of oven dry can obtain the polystyrene target capsule of fusion that diameter is 500 μ m wall thickness 15 μ m.
Embodiment bis-: the preparation method of the polystyrene target capsule of fusion of diameter 1000 μ m wall thickness 20 μ m
1. the preparation of passage:
1.. by three length of Peek threeway connection of an internal diameter 500 μ m, be that 15cm internal diameter is the Teflon pipe of 500 μ m, wherein No. 6 syringe needles are inserted respectively as capsule heart solution (water) entrance and capsule wall solution (polystyrene solution) entrance in one end of two tubes;
2.. another root does not have the outside of the Teflon pipe of pin to put the Teflon pipe of one section of internal diameter, 1000 μ m, the Teflon that stainless steel threeway by internal diameter 1000 μ m connects the long 1000 μ m internal diameters of other two 15cm manages, and insert in one end of a central Teflon pipe No. 6 syringe needles that put one section of internal diameter, 500 μ mTeflon pipes, as the entrance of mobile phase (polyvinyl alcohol water solution);
2. the preparation of microemulsion:
1.. 3.5g polystyrene (PS) is dissolved in to 25ml benzene and 25ml1, in the mixed solution of 2-ethylene dichloride, forms 7%PS solution;
2. .25g polyvinyl alcohol (PVA) (PVA) is dissolved in the middle of 500ml ultrapure water, forms 5%PVA solution;
3.. by water, PS solution, PVA solution sucks respectively syringe, is loaded on digital control syringe pump, and the syringe of three-phase connects respectively the capsule heart solution entrance, capsule wall solution entrance and mobile phase entrance.
4.. at software interface, setting pellet material is polystyrene; Solvent is benzene and 1,2-ethylene dichloride (1:1); Concentration is 7%; Required pellet diameter is 1000 μ m, wall thickness 20 μ m.System is set three-phase flow velocity according to prevalue: the flow velocity of water is 5ml/h, and the flow velocity of PS solution is 5ml/h, and the flow velocity of PVA solution is 80ml/h.Then start emulsion generation system, when the first water (water) is when first node place and oil phase (PS solution) meet, form monodispersed water-in-oil emulsion; While meeting by second node and the second water (PVA solution) again, formed again monodispersed water-in-oil-in-water compositions.
5.. control system gathers the image of microemulsion and calculates external diameter and the internal diameter of double emulsion, according to the relation between the internal-and external diameter value of the microemulsion calculating and they and three-phase solution flow rate, automatically regulate three-phase solution flow rate until the internal-and external diameter of microemulsion reaches the size requiring in advance.When the microemulsion of outlet is stablized, with the 500ml round-bottomed flask that 250mlPVA solution is housed, receive.
3. the preparation of target capsule of fusion
1.. after receiving the microemulsion of some, round-bottomed flask is placed in to Rotary Evaporators, set temperature is 60 ℃, and rotating speed is 40rpm, starts rotation;
2.. when microemulsion is dry, emerge, temperature is made as to 70 ℃, rotating speed is adjusted to 60rpm;
3.. at the bottom of microemulsion sinks to bottle again, temperature is made as to 80 ℃, rotating speed is adjusted to 80rpm, maintains 1h;
4.. the solvent for the treatment of PS solution evaporates completely, takes out microballoon, cleans and removes surperficial PVA solution, and 60 ℃ of oven dry can obtain the polystyrene target capsule of fusion that diameter is 500 μ m wall thickness 15 μ m.
Embodiment tri-: the preparation method of foam resin (RF/PF) target capsule of fusion of diameter 500 μ m wall thickness 20 μ m
1. the preparation of passage:
1.. a length, be that 15cm internal diameter is to stamp an aperture on the Teflon tube wall of 500 μ m, insert No. 6 medical needles that polish in advance, attention will be inserted in syringe needle the centre of pipe, and this syringe needle is as the entrance of capsule heart solution (1-methylnaphthalene);
2. No. 6 syringe needles are inserted in one end of .Teflon pipe, as the entrance of capsule wall solution (phenol resin solution);
3.. with the Peek threeway of internal diameter 500 μ m, connect the other end of this Teflon pipe and the Teflon pipe of the long 500 μ m internal diameters of other two 15cm, and insert No. 6 syringe needles in one end of a central Teflon pipe, as the entrance of mobile phase (mixing silicone oil).
2. the preparation of microemulsion:
1.. 5.72g resorcinol is dissolved in 54ml ultrapure water, adds 7.8ml37% formalin, 0.028g2.8wt%Na 2cO 3solution, agitating heating 1h under 70 ℃ of water-baths, puts into ice-water bath cooling, obtains RF solution;
2. .2.5g2,4,6-trihydroxybenzoic acid is dissolved in 24ml ultrapure water and adds 5ml1MNaOH solution 70 ℃ of mixing, then adds 3.43ml37% formalin at 70 ℃ of stirred in water bath heating 1h, puts into ice-water bath cooling, obtains PF solution;
3.. above two kinds of solution are mixed, obtain our required RF/PF mixed solution, as aggressiveness before cyst wall;
4.. 10cst silicone oil and fluorinated silicone oil are mixed according to 1:1 volume ratio, as mobile phase;
5.. by 1-methylnaphthalene, RF/PF solution, mix silicone oil and suck respectively syringe, be loaded on digital control syringe pump, the syringe of three-phase connects respectively the capsule heart solution entrance, capsule wall solution entrance and mobile phase entrance.
6.. at software interface, setting pellet material is RF/PF mixed solution; Required pellet diameter is 500 μ m, wall thickness 20 μ m.System is set three-phase flow velocity according to prevalue: the flow velocity of 1-methylnaphthalene is 2ml/h, and the flow velocity of RF/PF solution is 0.5ml/h, and the flow velocity that mixes silicone oil is 10ml/h.Then start emulsion generation system, when the first oil phase (1-methylnaphthalene) is when first node place and water (RF/PF solution) meet, form monodispersed O/w emulsion; While meeting with the second oil phase (mixing silicone oil) by second node again, formed again monodispersed Water-In-Oil bag fat liquor.
7.. control system gathers the image of microemulsion and calculates external diameter and the internal diameter of double emulsion, according to the relation between the internal-and external diameter value of the microemulsion calculating and they and three-phase solution flow rate, automatically regulate three-phase solution flow rate until the internal-and external diameter of microemulsion reaches the size requiring in advance.When the microemulsion of outlet is stablized, with being housed, the 500ml round-bottomed flask of 250ml containing the mixing silicone oil of 0.39% acetic acid receive.
3. the preparation of target capsule of fusion
1.. after receiving the microemulsion of some, round-bottomed flask is placed in to Rotary Evaporators, in 5min, rotating speed is risen to 95rpm, after 5min, be raised to 120rpm and continue 1min, return 95rpm and keep 50min to complete by catalyzed polymerization;
2.. take out phenolic resin microspheres, with normal hexane, wash away surperficial silicone oil and inner 1-methylnaphthalene;
3.. by alcohol gradient, displace the water in phenolics tiny balloon, then displace alcohol with isoamyl acetate;
4.. the phenolics tiny balloon being soaked in isoamyl acetate is dried in CO2 supercritical fluid, finally obtains foam resin target capsule of fusion.

Claims (2)

1. the target capsule of fusion preparation method based on microfluid, it is characterized in that, this preparation method based on emulsion automatic creation system comprise the chip that generates microemulsion, the syringe pump that fluid flow is controlled, the imaging system of microemulsion size observation, graphical analysis and flow control system: adopt microfluidic channel network to make pellet solution or front aggressiveness in mobile phase, form dual microemulsion, the pattern of double emulsion sends control system to by imaging system and carries out the internal-and external diameter that graphical analysis obtains double emulsion, then by flow control system, regulate the flow of each syringe pump to realize the control of double emulsion internal-and external diameter, thereby realize the diameter of hollow pellet, wall thickness is controlled, its concrete preparation method comprises the following steps:
1) preparation of microfluidic channel: adopt micro-processing technology to set up microfluidic channel network system on silicon chip, glass, polymethylmethacrylate or dimethyl silicone polymer micro-fluid chip, this system has 3 entrances, be respectively capsule heart phase entrance, cyst wall phase entrance, mobile phase entrance, have 1 outlet;
2) preparation of microemulsion: capsule heart phase, cyst wall phase, mobile phase three-phase solution are respectively charged into three syringes, are connected respectively 3 described entrances, control three-phase solution flow rate with digital control syringe pump, obtain uniform and stable microemulsion from outlet;
3) obtaining of microemulsion size: observe the generation situation of microemulsion by imaging system, the image of Real-time Collection microemulsion, goes out external diameter and the internal diameter of double emulsion by image analysis calculation;
4) control of double emulsion internal-and external diameter: the relation according between the internal-and external diameter value of the microemulsion calculating and they and three-phase solution flow rate, regulates three-phase solution flow rate automatically until the internal-and external diameter of microemulsion reaches the size precomputing;
5) preparation of target capsule of fusion: by microemulsion cyst wall dry solidification, remove capsule heart phase, obtain satisfactory hollow target capsule of fusion.
2. the target capsule of fusion preparation method based on microfluid according to claim 1, is characterized in that microfluidic channel network system is 2 grades of T-shaped channel patterns, or converges shearing channel pattern.
CN201410342972.9A 2014-07-17 2014-07-17 Method for manufacturing fusion pellet based on microfluid Pending CN104091620A (en)

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CN105013547A (en) * 2015-07-30 2015-11-04 天津大学 Novel microbubble/liquid drop generation regulation and control device and novel microbubble/liquid drop generation regulation and control method
CN105107558A (en) * 2015-09-14 2015-12-02 安徽博微长安电子有限公司 Full-automatic droplet formation system and control method thereof
CN109453706A (en) * 2018-11-15 2019-03-12 东南大学 A kind of preparation facilities of concentricization double emulsion
CN114307708A (en) * 2022-01-07 2022-04-12 苏州大学 Method for continuously preparing drug-loaded nano-emulsion

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105013547A (en) * 2015-07-30 2015-11-04 天津大学 Novel microbubble/liquid drop generation regulation and control device and novel microbubble/liquid drop generation regulation and control method
CN105107558A (en) * 2015-09-14 2015-12-02 安徽博微长安电子有限公司 Full-automatic droplet formation system and control method thereof
CN109453706A (en) * 2018-11-15 2019-03-12 东南大学 A kind of preparation facilities of concentricization double emulsion
CN109453706B (en) * 2018-11-15 2021-02-02 东南大学 Preparation facilities of double emulsion of concentricity
CN114307708A (en) * 2022-01-07 2022-04-12 苏州大学 Method for continuously preparing drug-loaded nano-emulsion

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Application publication date: 20141008