CN111978073A - Device and method for preparing crescent ceramic particles based on micro-fluidic chip and application - Google Patents
Device and method for preparing crescent ceramic particles based on micro-fluidic chip and application Download PDFInfo
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- CN111978073A CN111978073A CN202010922389.0A CN202010922389A CN111978073A CN 111978073 A CN111978073 A CN 111978073A CN 202010922389 A CN202010922389 A CN 202010922389A CN 111978073 A CN111978073 A CN 111978073A
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- glass tube
- crescent
- dispensing needle
- needle head
- phase fluid
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- 239000000919 ceramic Substances 0.000 title claims abstract description 67
- 239000002245 particle Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000012071 phase Substances 0.000 claims abstract description 72
- 239000011521 glass Substances 0.000 claims abstract description 68
- 239000008385 outer phase Substances 0.000 claims abstract description 40
- 239000008384 inner phase Substances 0.000 claims abstract description 28
- 239000011859 microparticle Substances 0.000 claims description 74
- 239000012530 fluid Substances 0.000 claims description 60
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 26
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 16
- 239000002105 nanoparticle Substances 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 12
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 10
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 9
- 239000004094 surface-active agent Substances 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000004132 cross linking Methods 0.000 claims description 6
- 229920002545 silicone oil Polymers 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000010008 shearing Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims description 3
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 239000000499 gel Substances 0.000 description 8
- 239000003921 oil Substances 0.000 description 6
- 238000001723 curing Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004005 microsphere Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000002003 electron diffraction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000000520 microinjection Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 229960000074 biopharmaceutical Drugs 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012837 microfluidics method Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000879 optical micrograph Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
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Abstract
The invention relates to a device, a method and application for preparing crescent ceramic particles based on a microfluidic chip, wherein the device comprises a bottom plate, a first dispensing needle head, a second dispensing needle head, an inner phase glass tube, an outer phase glass tube, an ultraviolet lamp holder and a collection hose; the first dispensing needle head and the second dispensing needle head are fixed on the bottom plate in parallel, one port of the inner phase glass tube is communicated with the cavity of the first dispensing needle head, one port of the outer phase glass tube is communicated with the cavity of the second dispensing needle head, and the other port of the inner phase glass tube penetrates through the cavity of the second dispensing needle head and then extends into the outer phase glass tube; the ultraviolet lamp holder is arranged above the external phase glass tube, and the other port of the external phase glass tube is fixedly connected with the collection hose and is communicated with the inner space of the collection hose.
Description
Technical Field
The invention relates to the technical field of ceramic microparticle preparation, in particular to a device and a method for preparing crescent ceramic particles based on a microfluidic chip and application of the crescent ceramic particles.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
The ceramic material has better high temperature resistance, wear resistance and chemical corrosion resistance, and excellent mechanical property, so that the ceramic material becomes a substitute of various metals or alloys in the industrial field. The ceramic microparticles not only have the general properties of ceramic materials, but also conform to the development trend of miniaturization and precision of the using habitat of parts. With the development of abrasives, sensors, electromagnetic components, biopharmaceuticals, nuclear fuel elements, micro-components of micro-electro-mechanical systems, etc., ceramic microparticles show unprecedented prospects for development. There are many factors that affect the performance of ceramic microparticles, and shape is one of the important factors. The ceramic microparticles have both spherical and non-spherical shapes, and the microspheres prepared by the traditional methods for preparing spherical ceramic microparticles, such as spray drying, fluidized bed granulation, rotary shearing granulation, vibration dispersion and the like, have uneven sizes and cannot be accurately controlled; methods for preparing non-spherical ceramic microparticles such as gel casting, powder microinjection molding, and microinjection molding often depend on a mold, and have poor adjustability; micro stereolithography (μ SL) can produce ceramic particles in three-dimensional shapes but with low production efficiency.
The microfluid technology provides a continuous and adjustable way to prepare spherical and non-spherical ceramic microparticles, and the prepared microparticles have good monodispersity and higher yield. The microfluidics method of the droplet template is applied to the preparation of spherical ceramic microparticles in combination with the processes of inner and outer gels; another microfluid molding method, fluid lithography molding, is applied to the production of non-spherical ceramic microparticles, but the inventors found that the shapes of the ceramic microparticles prepared by the above preparation method are mostly two-dimensionally stretched shapes, and the materials are mostly limited to silicon oxide; therefore, a relatively simple, continuous, and controllable method for preparing non-spherical ceramic microparticles with three-dimensional structural characteristics has not been provided so far.
Disclosure of Invention
Aiming at the technical problems, the invention aims to provide a device, a method and application for preparing crescent ceramic particles based on a microfluidic chip. The method comprises the steps of respectively introducing a water phase precursor in which ceramic nanoparticles and photo-initiation prepolymer are dispersed and a surfactant is dissolved and an oil phase in which the surfactant is dissolved into an inner phase glass tube and an outer phase glass tube in a micro-fluidic chip, wherein at the outlet of the inner phase glass tube, the inner water phase forms water-in-oil droplets under the action of shearing force of the outer oil phase, the droplets are subjected to cross-linking polymerization reaction at a downstream ultraviolet light position, and the crescent ceramic microparticles obtained after cleaning, aging, drying and sintering have the characteristics of obvious three-dimensional shape characteristics, accurate and adjustable shape and uniform size.
The first object of the present invention: provides a device for preparing crescent ceramic particles based on a microfluidic chip.
The second object of the present invention: a method for preparing crescent ceramic particles based on a microfluidic chip is provided.
The third object of the present invention: provides the application of the method for preparing crescent ceramic particles based on the microfluidic chip.
In order to realize the purpose, the invention discloses the following technical scheme:
the invention discloses a device for preparing crescent ceramic particles based on a microfluidic chip, which comprises a bottom plate, a first dispensing needle head, a second dispensing needle head, an inner phase glass tube, an outer phase glass tube, an ultraviolet lamp holder and a collection hose; the first dispensing needle head and the second dispensing needle head are fixed on the bottom plate in parallel, one port of the inner phase glass tube is communicated with the cavity of the first dispensing needle head, one port of the outer phase glass tube is communicated with the cavity of the second dispensing needle head, and the other port of the inner phase glass tube penetrates through the cavity of the second dispensing needle head and then extends into the outer phase glass tube; the ultraviolet lamp holder is arranged above the outer-phase glass tube, and the other port of the outer-phase glass tube is fixedly connected with the collection hose and communicated with the inner space of the collection hose.
Secondly, the invention discloses a method for preparing crescent ceramic particles based on a microfluidic chip, which comprises the following steps:
introducing the external phase fluid into the second dispensing needle head, then entering the external phase glass tube, and introducing the internal phase fluid through the first dispensing needle head and the internal phase glass tube when the external phase fluid flows out of the outlet of the external phase glass tube;
the outer phase fluid forms liquid drops coated by the outer phase fluid at the outlet of the inner phase glass tube under the action of the shearing force of the outer phase fluid, and the liquid drops flow through the ultraviolet exposure area and flow into the collection hose along with the outer phase fluid after exposure and solidification;
and cleaning the collected liquid drops, respectively removing the external phase fluid and the uncured internal phase solution, standing the obtained crescent-shaped microparticles in an ammonium persulfate aqueous solution, further performing crosslinking ageing in an environment of 60-70 ℃, drying the crosslinked and aged particles, and then sintering the particles at a high temperature to obtain the crescent-shaped ceramic microparticles.
Further, the internal phase fluid is a slurry solution mixed with acrylamide monomer, N '-methylene bisacrylamide, photoinitiator 1173, alumina nano-dispersion, the concentration of alumina nano-particles in the internal phase fluid is fixed at 70-71 wt.%, preferably 70.7 wt.%, the concentration of acrylamide monomer is fixed at 7.0-7.6 wt.%, preferably 7.3 wt.%, and the concentration of N, N' -methylene bisacrylamide is fixed at 1.0-1.4 wt.%; preferably 1.2 wt.%, and the concentration of photoinitiator 1173 is from 3 to 5 vt.%, preferably 4 vt.%.
Further, the external phase fluid is a silicone oil solution dissolved with a surfactant EM 90, and the concentration of the surfactant EM 90 is 1-3 vt%, preferably 2.0 vt%.
Compared with the prior art, the preparation method and the formula of the crescent ceramic micro-particles have the following beneficial effects in the aspect of performance:
(1) the preparation method is based on the microfluid chip, and the crescent-shaped gel microparticles prepared by oil-water two-phase have the characteristics of precise and controllable shape and uniform size, and provide a foundation for batch stable production of the crescent-shaped gel microparticles.
(2) According to the invention, the alumina nano dispersion liquid is obtained by grinding, and the characteristic of the alumina nano particles in absorbing and scattering ultraviolet light is utilized, so that the crescent colloid micro particles and the deformed micro particles thereof are prepared by the slurry micro-droplets. Nanoparticles based on a wide range of ceramic materials all have the property of absorbing and scattering light, and the method has a guiding role in the preparation of crescent-shaped ceramic microparticles coated with materials such as zirconia, silicon nitride, silicon carbide and the like.
(3) The device and the method can be used for continuously preparing the special-shaped gel microparticles in one step, so that the subsequent preparation of the special-shaped ceramic microparticles is separated from the traditional die, the steps are simple and easy to implement, and the production efficiency is high.
(4) According to the invention, crescent-shaped gel microparticles with different thicknesses can be prepared by adjusting the light intensity of the ultraviolet lamp, and crescent-shaped and deformed gel microparticles with different lengths can be prepared by adjusting the ratio of oil phase to water phase.
(5) According to the invention, the crescent-shaped gel microparticles are sintered at high temperature, wherein the coated alumina nanoparticles can be mutually bonded to form crescent-shaped ceramic microparticles with higher strength through further high-temperature treatment. The special-shaped ceramic microparticles prepared by the device and the method can be applied to micro-robots, micro-electro-mechanical system components, biological materials and the like.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
FIG. 1 is a schematic view of the overall structure of embodiment 1 of the present invention;
FIG. 2 is a schematic flow chart of a method according to embodiment 4 of the present invention;
FIG. 3 is an optical microscope image of the reflection and transmission of slurry microsphere droplets containing crescent-shaped colloidal microparticles obtained in example 4 of the present invention;
FIG. 4 is a scanning electron microscope photograph of crescent-shaped colloidal microparticles prepared under different UV light intensity conditions in example 5 of the present invention;
FIG. 5 is a scanning electron microscope photograph of crescent-shaped deformed colloidal microparticles prepared under different external phase to internal phase flow rate conditions according to example 6 of the present invention;
FIG. 6 is a scanning electron microscope photograph of ceramic microparticles obtained after sintering of crescent-shaped microspheres prepared in example 4 of the present invention;
FIG. 7 is a transmission electron microscope lattice fringe image, an electron diffraction image and an XRD characterization image of crescent-shaped microparticles obtained by sintering in example 4 of the present invention;
FIG. 8 is a scanning electron microscope photograph of microparticles prepared in comparative example 1 of the present invention;
FIG. 9 is an optical microscope photograph of microparticles prepared in comparative example 2 of the present invention;
the device comprises a base plate 1, a first dispensing needle head 2, an inner phase glass tube 3, a second dispensing needle head 4, an outer phase glass tube 5, an ultraviolet lamp head 6 and a collection hose 7.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As described in the background art, most of the ceramic microparticles prepared by the existing ceramic microparticle preparation method are in two-dimensional stretching shapes, and most of the materials are limited to silicon oxide.
In one exemplary embodiment of the present application, the preparation method comprises the steps of:
introducing an external phase fluid into a second dispensing needle head, then introducing the external phase fluid into an external phase glass tube, and introducing an internal phase fluid through a first dispensing needle head and an internal phase glass tube when the external phase fluid flows out of an outlet of the external phase glass tube;
forming liquid drops coated by the outer phase fluid at the outlet of the inner phase glass tube by the inner phase fluid due to the shearing force of the outer phase fluid, wherein the liquid drops flow through the ultraviolet exposure area and flow into a collection hose along with the outer phase fluid after exposure and solidification;
and (3) cleaning the collected droplets, respectively removing the external phase fluid and the uncured internal phase solution, standing the obtained crescent-shaped microparticles in an ammonium persulfate aqueous solution for further crosslinking and aging at the temperature of 60-70 ℃, drying to obtain crescent-shaped colloidal microparticles, and sintering at high temperature to obtain the crescent-shaped ceramic microparticles. Preferably, the obtained crescent-shaped microparticles are stood in an aqueous ammonium sulfate solution for further crosslinking and aging at 65 ℃.
In the step (1), the internal phase fluid is a slurry solution mixed with acrylamide monomer, N' -methylene bisacrylamide, a photoinitiator 1173 and alumina nano dispersion liquid; the external phase fluid is a silicone oil solution of EM 90;
specifically, the concentration of alumina nanoparticles in the internal phase fluid is fixed at 70-71 wt.%, preferably 70.7 wt.%, the concentration of acrylamide monomer is fixed at 7.0-7.6 wt.%, preferably 7.3 wt.%, and the concentration of N, N' -methylenebisacrylamide is fixed at 1.0-1.4 wt.%; preferably 1.2 wt.%, the concentration of photoinitiator 1173 is from 3 to 5 vt.%, preferably 4 vt.%, and the concentration of surfactant EM 90 in the external phase fluid is from 1 to 3 vt.%, preferably 2.0 vt.%.
The inventor finds that the alumina nano-particles play a structural role of supporting the crescent shape, the concentration of the alumina nano-particles is too low, and the crescent micro-particles prepared subsequently are shrunk in the drying process, so that the strength is reduced after sintering. The alumina nano-particle concentration is too high, the curing difficulty is increased, stronger ultraviolet intensity is needed, and the equipment investment is increased.
Specifically, the preparation method of the alumina nano dispersion liquid comprises the following steps: aluminum oxide powder with the particle size of 1 mu m and the purity of 99.99 percent is weighed, 0.8 to 1.2 weight percent of ammonium citrate dispersant is added, then the mixture is dissolved in water, preferably deionized water, and the mixture is ball-milled in a ball mill for 12 to 36 hours, preferably 1.0 weight percent of ammonium citrate dispersant, and the ball-milling time is preferably 24 hours.
Specifically, the preparation method of the slurry solution comprises the following steps: mixing and oscillating acrylamide powder, N, N' -methylene bisacrylamide powder, a photoinitiator 1173 and the alumina nano dispersion liquid to obtain the nano-composite material.
Wherein the mass-to-volume ratio of the acrylamide powder, the N, N' -methylene bisacrylamide powder, the photoinitiator 1173 and the alumina nano dispersion liquid is as follows: 0.15-0.25 g: 0.03-0.36 g: 10-100 ul: 0.8-1.2 mL; preferably 0.2 g: 0.033 g: 50 ul: 1 ml.
The external phase fluid is obtained by mixing and oscillating silicone oil and a surfactant EM 90, and the volume ratio of the silicone oil to the surfactant is as follows: 8-12:0.1-0.3, preferably 10: 0.2.
Specifically, in the step (3), the preparation method of the ammonium persulfate solution comprises the following steps: ammonium persulfate solid powder is weighed and added to water to 1-5 wt.%, preferably 3 wt.%, with shaking for 10 seconds-1 minute, preferably 30 seconds. Preferably, ammonium persulfate fixed powder is added to deionized water and shaken.
The ultraviolet curing of the opaque liquid drops is one of key technologies, and in the existing method for preparing microparticles based on the ultraviolet curing of the incompletely transparent photopolymerizable solution used in microfluidics, the content of dispersed nanoparticles in the incompletely transparent precursor solution is relatively low, which causes the prepared microparticles to have low strength and limited application. In this embodiment, the ultraviolet curing method is combined with the ceramic slurry, and the ultraviolet exposure is performed after the aqueous phase droplets are stably generated, and because the aluminum oxide nanoparticles in the slurry droplets absorb and reflect the ultraviolet light, the ultraviolet light can only penetrate through a limited depth, so that crescent-shaped and deformed colloidal microparticles thereof are prepared by the droplet template, and then the ceramic microparticles are obtained by sintering.
In some exemplary embodiments, in step (1), the total fixed internal and external phase fluid flow rate is 44 μ L/min; the inner phase flow rate ranges from 1 to 11. mu.L/min and the outer phase flow rate ranges from 43 to 33. mu.L/min. The difference in the flow rate ratio of the outer and inner phases results in the difference in the aspect ratio and the shape of the non-spherical colloidal microparticles obtained after uv curing. Therefore, in this embodiment, crescent-shaped deformed microparticles with different aspect ratios are obtained by controlling the flow rate ratio of the outer phase and the inner phase.
In some exemplary embodiments, the ultraviolet light of different intensities in step (2) has different capabilities of passing through the opaque alumina nanoparticles with light intensities ranging from 1-6mW/cm2The colloidal particles with different thicknesses can be collected and obtained. Specifically, the light intensity may be 1.26mW/cm2，2.14mW/cm2，3.40mW/cm2And 5.36mW/cm2。
In some exemplary embodiments, in step (3), the slurry droplets containing crescent-shaped microparticles are sequentially washed in petroleum ether and deionized water for removing the external phase fluid and the internal phase fluid which is not uv-cured, respectively; the method specifically comprises the following steps: and after the petroleum ether is fully volatilized, deionized water is added to remove the slurry solution which is not photocured, and after the cleaning solution is clarified, the deionized water is sucked to be dried to obtain crescent colloidal microparticles.
In some typical examples, in step (3), the crosslinking and aging time is not less than 1h by using ammonium persulfate solution, so that the acrylamide monomer which is not completely crosslinked inside the microparticles is fully crosslinked and aged. After aging, collecting colloid microparticles, and drying on a Teflon film at normal temperature for 6-18 hours, preferably for 12 hours.
In some typical embodiments, in the step (3), the high-temperature sintering is performed by firstly burning off organic matters such as polyacrylamide and the like in a step heating manner, and then heating and bonding the alumina nanoparticles to form an alumina ceramic structure; the method specifically comprises the following steps: heating at 1 deg.C/min before 600 deg.C, respectively maintaining at 115 deg.C, 234 deg.C, 236 deg.C, 373 deg.C, 375 deg.C, 496 deg.C and 600 deg.C for 1 hr, heating at 5 deg.C/min to 1549 deg.C and 1551 deg.C after 600 deg.C, maintaining at 1550 deg.C for 2 hr, and cooling to room temperature with the furnace.
In some exemplary embodiments, the crescent-shaped ceramic microparticles prepared by the above method and the apparatus for preparing crescent-shaped ceramic microparticles based on a microreactor are used in the fields of micro-robots, micro-electromechanical systems, and biotechnology.
The invention will now be further described with reference to the accompanying drawings and detailed description.
Example 1:
as shown in fig. 1, an apparatus for preparing crescent-shaped ceramic particles based on a microfluidic chip includes: the device comprises a bottom plate 1, a first dispensing needle head 2, an inner phase glass tube 3, a second dispensing needle head 4, an outer phase glass tube 5, an ultraviolet lamp holder 6 and a collection hose 7; the first dispensing needle head 2 and the second dispensing needle head 4 are fixed on the bottom plate 1 side by side, one port of the inner phase glass tube 3 is communicated with the cavity of the first dispensing needle head 2, one port of the outer phase glass tube 5 is communicated with the cavity of the second dispensing needle head 4, and the other port of the inner phase glass tube 3 passes through the cavity of the second dispensing needle head 4 and then extends into the outer phase glass tube 5; the ultraviolet lamp holder 6 is arranged right above the outer-phase glass tube 5 and can be connected with an ultraviolet lamp source, and the other end of the outer-phase glass tube 5 is connected with the collection hose 7 and is fixed in an interference fit manner.
It should be noted that the apparatus of the present embodiment has the following features:
(1) compared with the current PDMS channel chip, the equipment has low cost, and the average cost of each chip is less than one yuan;
(2) the size of the crescent colloidal microparticles is determined by the size of the droplets, the size of the droplets is determined by the inner diameter of the capillary, and the capillaries with different inner diameters can be freely replaced to control the maximum size of the crescent colloidal microparticles; therefore, expansion can be carried out on the basis of regulating the size of the microspheres by the flow rate;
(3) the operation process is visualized, and the generation condition of the liquid drops can be clearly observed on the glass chip without a microscope.
Example 2:
an apparatus for preparing crescent ceramic particles based on a microfluidic chip, which is the same as example 1, except that: the device is characterized by further comprising injectors for injecting the internal phase fluid and the external phase fluid respectively, wherein the first dispensing needle head 2 and the second dispensing needle head 4 are connected with one injector respectively, and the injectors are driven by flow pumps so as to inject the internal phase fluid and the external phase fluid into the first dispensing needle head 2 and the second dispensing needle head 4 respectively.
Example 3:
an apparatus for preparing crescent ceramic particles based on a microfluidic chip, which is the same as example 2, except that: the bottom plate is a 7101 type glass slide, the inner phase glass tube 3 and the outer phase glass tube 5 are capillary glass tubes with the length of 50mm, the inner diameter of the inner phase glass tube 4 is 0.13mm, and the inner diameter of the outer phase glass tube 5 is 0.6 mm. The inner phase glass tube 4 and the outer phase glass tube 5 are fixed with the glass slide by gluing.
Example 4:
as shown in fig. 2 to 3, a method for preparing crescent-shaped ceramic particles based on a microfluidic chip comprises the following steps:
step 1: preparing an alumina nano dispersion liquid: weighing 19.5g of alumina powder, 0.195g of ammonium citrate and 5g of deionized water, mixing, and ball-milling for 24 hours at 450 revolutions per minute in a planetary ball mill to obtain alumina dispersion liquid with the volume ratio of the alumina powder being 50%.
Step 2: preparation of slurry liquid: 0.2g of acrylamide, 0.033g N, N' -methylenebisacrylamide, 50. mu.L of photoinitiator 1173 and 1mL of the alumina nanodispersion described in step 1 of example 4 were weighed and mixed and vortexed for 5 minutes to provide an internal phase fluid having an alumina nanoparticle concentration of 70.7 wt%.
And step 3: preparing an external phase fluid: 10mL of silicone oil and 0.2mL of EM 90 are weighed and mixed, and vortex oscillation is carried out for 5 minutes, so as to obtain the external phase fluid.
And 4, step 4: using the prepared internal phase fluid and external phase fluid, crescent-shaped ceramic microparticles were prepared using the apparatus described in example 3, specifically:
step a: introducing the prepared external phase fluid into a second dispensing needle through an injector, and then entering an external phase glass tube; when the external phase fluid flows out of the outlet, the prepared internal phase fluid in the embodiment is introduced into the first dispensing needle head through the injector and then enters the external phase glass tube, the flow rates of the internal phase fluid and the external phase fluid are respectively 4 muL/min and 40 muL/min, and the light intensity of the ultraviolet lamp is 3.40mW/cm2And (4) carrying out the test.
Step b: the collecting hose is adopted to collect the slurry liquid drops and the external phase fluid and carry the slurry liquid drops and the external phase fluid into a plastic cup, a 1mL dropper is used for sucking silicon oil and then adding petroleum ether for multiple times of cleaning, and after the petroleum ether is completely volatilized, deionized water is used for multiple times of cleaning to remove the uncured slurry liquid. The solidified microparticles are collected and placed in an ammonium persulfate aqueous solution, and aged for 1 hour in an environment of 65 ℃.
The preparation method of the ammonium persulfate aqueous solution comprises the following steps: ammonium persulfate solid powder was weighed, added to deionized water to reach 3 wt.%, and shaken for 30 seconds.
Step c: after the microparticles are aged, they are dried on teflon film for 12 hours, and the average particle size of the microparticles is reduced.
Step d: after drying, putting the colloidal microparticles into a sintering furnace, heating to 600 ℃ from room temperature at 1 ℃/min, and then heating to 1550 ℃ at 5 ℃/min; wherein the temperature is respectively kept at 114 ℃,235 ℃,374 ℃,495 ℃ and 600 ℃ for 1 hour, and at 1550 ℃ for 2 hours, and then the crescent ceramic microparticles can be obtained after furnace cooling, as shown in figures 6 to 7.
Fig. 6 is a scanning electron microscope image of the ceramic microparticles obtained after sintering. Fig. 6(a), 6(b), and 6(c) are respectively an overall view of the sintered ceramic fine particles, enlarged views of two ceramic fine particles, and further enlarged images of the surface crystal grains of the ceramic obtained from the ceramic structure.
FIG. 7 is a representation of the ceramic structure of crescent-shaped microparticles after sintering. Fig. 7(a), 7(b), and 7(c) are transmission electron microscope lattice fringe images, electron diffraction images, and XRD identification images of the ceramic microparticles, respectively.
Example 5:
as shown in fig. 4, a method for preparing crescent-shaped ceramic microparticles based on a microfluidic chip is similar to example 4, except that: the light intensity of the ultraviolet lamp is 1.26mW/cm2，2.14mW/cm2，3.40mW/cm2，5.36mW/cm2And (4) preparation.
Example 6:
as shown in fig. 5, a method for preparing crescent ceramic particles based on a microfluidic chip is the same as that in example 4, except that: the light intensity of the ultraviolet lamp is fixed to be 3.40mW/cm2The flow rate of the fluid in the internal phase is sequentially changed from 11 μ L/min to 1 μ L/min with a gradient of 1 μ L/min, i.e., the flow rate ratio (Q) between the external phase and the internal phaseOil：QSlurry material) From 3 to 43.
Comparative example 1:
as shown in fig. 8, crescent-shaped microparticles obtained by cleaning with petroleum ether and deionized water without aging with ammonium persulfate solution are directly collected from the collection hose, and are directly dried and sintered, wherein the shape of the crescent-shaped microparticles is as shown in fig. 8, the deformation of the edge and the concave surface is large, the strength is low, the microparticles are mutually bonded in the drying process, and crescent-shaped colloidal microparticles with good shape quality and good monodispersity cannot be obtained.
Comparative example 2:
as shown in FIG. 9, the internal phase fluid, formulated with a dispersion of aluminum oxide powder having a solids content of 20 vt%, was 5.36mW/cm2The micro-particles prepared under the ultraviolet irradiation condition have shrinkage and collapse, and the crescent shape is difficult to distinguish.
Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the present invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive efforts by those skilled in the art based on the technical solution of the present invention.
Claims (10)
1. The device for preparing crescent ceramic particles based on the microfluidic chip is characterized by comprising a bottom plate, a first dispensing needle head, a second dispensing needle head, an inner phase glass tube, an outer phase glass tube, an ultraviolet lamp holder and a collection hose; the first dispensing needle head and the second dispensing needle head are fixed on the bottom plate in parallel, one port of the inner phase glass tube is communicated with the cavity of the first dispensing needle head, one port of the outer phase glass tube is communicated with the cavity of the second dispensing needle head, and the other port of the inner phase glass tube penetrates through the cavity of the second dispensing needle head and then extends into the outer phase glass tube; the ultraviolet lamp holder is arranged above the outer-phase glass tube, and the other port of the outer-phase glass tube is fixedly connected with the collection hose and communicated with the inner space of the collection hose.
2. The apparatus for preparing crescent-shaped ceramic particles based on microfluidic chip of claim 1, further comprising injectors for injecting the inner phase fluid and the outer phase fluid, respectively, wherein the first dispensing needle and the second dispensing needle are connected to the injectors, respectively, and the injectors are connected to a flow pump.
3. The microfluidic chip-based apparatus for preparing crescent-shaped ceramic particles according to claim 1, wherein the base plate is a glass slide, the inner phase glass tube and the outer phase glass tube are capillary glass tubes with a length of 50-70mm, and the inner phase glass tube and the outer phase glass tube are fixedly connected to the glass slide.
4. A method for preparing crescent-shaped ceramic particles on the basis of a microfluidic chip, carried out using the device according to any one of claims 1 to 3, comprising the steps of:
introducing the external phase fluid into the second dispensing needle head, then entering the external phase glass tube, and introducing the internal phase fluid through the first dispensing needle head and the internal phase glass tube when the external phase fluid flows out of the outlet of the external phase glass tube;
the outer phase fluid forms liquid drops coated by the outer phase fluid at the outlet of the inner phase glass tube under the action of the shearing force of the outer phase fluid, and the liquid drops flow through the ultraviolet exposure area and flow into the collection hose along with the outer phase fluid after exposure and solidification;
and cleaning the collected liquid drops, respectively removing the external phase fluid and the uncured internal phase solution, standing the obtained crescent-shaped microparticles in an ammonium persulfate aqueous solution, further performing crosslinking ageing in an environment of 60-70 ℃, drying the crosslinked and aged particles, and then sintering the particles at a high temperature to obtain the crescent-shaped ceramic microparticles.
5. The method for preparing crescent-shaped ceramic particles based on a microfluidic chip according to claim 4, wherein the internal phase fluid is a slurry solution mixed with acrylamide monomer, N, N '-methylenebisacrylamide, photoinitiator 1173, and alumina nano-dispersion, the concentration of alumina nano-particles in the internal phase fluid is fixed at 70-71 wt.%, preferably 70.7 wt.%, the concentration of acrylamide monomer is fixed at 7.0-7.6 wt.%, preferably 7.3 wt.%, and the concentration of N, N' -methylenebisacrylamide is fixed at 1.0-1.4 wt.%; preferably 1.2 wt.%, and the concentration of photoinitiator 1173 is from 3 to 5 vt.%, preferably 4 vt.%.
6. The method for preparing crescent-shaped ceramic particles based on microfluidic chip according to claim 4, wherein the external phase fluid is a silicone oil solution dissolved with surfactant EM 90, and the concentration of surfactant EM 90 is 1-3 vt%, preferably 2.0 vt%.
7. The method for preparing crescent-shaped ceramic particles based on the microfluidic chip according to claim 4, wherein the specific method for high-temperature sintering comprises: heating at 1 deg.C/min before 600 deg.C, respectively maintaining at 115 deg.C, 236 deg.C, 373 deg.C, 375 deg.C, 494 deg.C, 496 deg.C and 600 deg.C for 1 hr, heating at 5 deg.C/min to 1549 deg.C and 1551 deg.C after 600 deg.C, maintaining for 2 hr, and cooling to room temperature with the furnace.
8. The method for preparing crescent-shaped ceramic particles based on a microfluidic chip according to claim 5, wherein the preparation method of the alumina nano dispersion liquid comprises the following steps: the alumina powder is added to 0.8-1.2 wt.% ammonium citrate dispersant, dissolved in water and ball milled for 12-36 hours.
9. The method for preparing crescent-shaped ceramic particles based on the microfluidic chip according to claim 1, wherein the ammonium persulfate solution is prepared by the following steps: weighing ammonium persulfate solid powder, adding into water to reach 1-5 wt.%, and shaking for 10 s-1 min.
10. Use of the apparatus for preparing crescent-shaped ceramic particles based on microfluidic chip according to any of claims 1-3 and/or crescent-shaped ceramic particles prepared by the method according to any of claims 4-9 in the fields of micro-robots, micro-electro-mechanical systems and biotechnology.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112829038A (en) * | 2021-01-06 | 2021-05-25 | 山东大学 | Ceramic microparticles of specific size using microfluidic chip, and apparatus, method and use thereof |
| CN115056479A (en) * | 2022-07-04 | 2022-09-16 | 南京周子未来食品科技有限公司 | Cell culture meat production equipment based on microfluidic 3D printing technology and application thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4016555C1 (en) * | 1990-05-23 | 1991-06-27 | Alfred 7500 Karlsruhe De Graentzel | Cooled UV-low pressure emitter esp. mercury vapour lamp - has extended discharge tube sub-divided into several longitudinal sections parallel to one another and bonded by means of elbows |
| CN1826170A (en) * | 2003-07-18 | 2006-08-30 | 巴克斯特国际公司 | Methods for fabrication, uses and compositions of small spherical particles of hgh prepared by controlled phase separation |
| EP2004316A2 (en) * | 2006-01-27 | 2008-12-24 | The President and Fellows of Harvard College | Fluidic droplet coalescence |
| US20100149259A1 (en) * | 2008-12-17 | 2010-06-17 | Robert Lee Cornell | Uv-curable coatings and methods for applying uv-curable coatings using thermal micro-fluid ejection heads |
| CN102311095A (en) * | 2011-08-09 | 2012-01-11 | 吉林大学 | Method for preparing multistage metal micro-nanostructures inside micro fluidic chip |
| CN102585252A (en) * | 2011-01-10 | 2012-07-18 | 中国科学院大连化学物理研究所 | Method for synthesizing nonspherical polymer microparticles |
| CN108285347A (en) * | 2018-02-12 | 2018-07-17 | 广东工业大学 | A kind of 3D printing photocuring ceramic particle and preparation method thereof |
| CN108827834A (en) * | 2018-08-03 | 2018-11-16 | 中国科学院力学研究所 | The acquisition methods of gas liquid film in a kind of micron capillary tube passage |
| CN109482111A (en) * | 2018-11-07 | 2019-03-19 | 四川大学 | The aspherical microparticle of bullet shaped and micro-capsule and preparation method thereof |
| CN110639450A (en) * | 2019-09-29 | 2020-01-03 | 山东大学 | Device and method for preparing calcium alginate microspheres by using microreactor and application of device |
| CN111572199A (en) * | 2019-02-19 | 2020-08-25 | 佳能株式会社 | Liquid ejection head, liquid ejection module, and method of manufacturing liquid ejection head |
-
2020
- 2020-09-04 CN CN202010922389.0A patent/CN111978073B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4016555C1 (en) * | 1990-05-23 | 1991-06-27 | Alfred 7500 Karlsruhe De Graentzel | Cooled UV-low pressure emitter esp. mercury vapour lamp - has extended discharge tube sub-divided into several longitudinal sections parallel to one another and bonded by means of elbows |
| CN1826170A (en) * | 2003-07-18 | 2006-08-30 | 巴克斯特国际公司 | Methods for fabrication, uses and compositions of small spherical particles of hgh prepared by controlled phase separation |
| EP2004316A2 (en) * | 2006-01-27 | 2008-12-24 | The President and Fellows of Harvard College | Fluidic droplet coalescence |
| US20100149259A1 (en) * | 2008-12-17 | 2010-06-17 | Robert Lee Cornell | Uv-curable coatings and methods for applying uv-curable coatings using thermal micro-fluid ejection heads |
| CN102585252A (en) * | 2011-01-10 | 2012-07-18 | 中国科学院大连化学物理研究所 | Method for synthesizing nonspherical polymer microparticles |
| CN102311095A (en) * | 2011-08-09 | 2012-01-11 | 吉林大学 | Method for preparing multistage metal micro-nanostructures inside micro fluidic chip |
| CN108285347A (en) * | 2018-02-12 | 2018-07-17 | 广东工业大学 | A kind of 3D printing photocuring ceramic particle and preparation method thereof |
| CN108827834A (en) * | 2018-08-03 | 2018-11-16 | 中国科学院力学研究所 | The acquisition methods of gas liquid film in a kind of micron capillary tube passage |
| CN109482111A (en) * | 2018-11-07 | 2019-03-19 | 四川大学 | The aspherical microparticle of bullet shaped and micro-capsule and preparation method thereof |
| CN111572199A (en) * | 2019-02-19 | 2020-08-25 | 佳能株式会社 | Liquid ejection head, liquid ejection module, and method of manufacturing liquid ejection head |
| CN110639450A (en) * | 2019-09-29 | 2020-01-03 | 山东大学 | Device and method for preparing calcium alginate microspheres by using microreactor and application of device |
Non-Patent Citations (4)
| Title |
|---|
| LIU QIAN 等: "Self-Orienting Hydrogel Micro-Buckets as Novel Cell Carriers", 《ANGEWANDTE CHEMIE》 * |
| SHIN-HYUN KIM 等: "Amphiphilic Crescent-Moon-Shaped Microparticles Formed by Selective Adsorption of Colloids", 《JOURNAL OF THE AMERICAN CHEMICAL SOCIETY》 * |
| ZHOU CHENCHEN 等: "Fabrication of crescent-shaped ceramic microparticles based on single emulsion microfluidics", 《CERAMICS INTERNATIONAL》 * |
| 刘一寰 等: "基于微流控技术制备微/纳米粒子材料", 《化学进展》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112829038A (en) * | 2021-01-06 | 2021-05-25 | 山东大学 | Ceramic microparticles of specific size using microfluidic chip, and apparatus, method and use thereof |
| CN112829038B (en) * | 2021-01-06 | 2022-03-08 | 山东大学 | Ceramic microparticles of specific size using microfluidic chip, and apparatus, method and use thereof |
| CN115056479A (en) * | 2022-07-04 | 2022-09-16 | 南京周子未来食品科技有限公司 | Cell culture meat production equipment based on microfluidic 3D printing technology and application thereof |
| CN115056479B (en) * | 2022-07-04 | 2024-01-23 | 南京周子未来食品科技有限公司 | Cell culture meat production equipment based on microfluidic 3D printing technology and application thereof |
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