CN110523449A - A kind of preparation method of crystalline ceramics micro-fluidic chip - Google Patents
A kind of preparation method of crystalline ceramics micro-fluidic chip Download PDFInfo
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- CN110523449A CN110523449A CN201910908949.4A CN201910908949A CN110523449A CN 110523449 A CN110523449 A CN 110523449A CN 201910908949 A CN201910908949 A CN 201910908949A CN 110523449 A CN110523449 A CN 110523449A
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- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502707—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by the manufacture of the container or its components
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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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
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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Abstract
The invention discloses a kind of preparation methods of crystalline ceramics micro-fluidic chip, this method designs to obtain the substrate model with very low power pattern first with modeling software, ceramic bases green compact are printed using ceramic photocuring technology, then by substrate green compact are degreasing sintered and transparence is realized in high temperature and pressure sintering；Transparent ceramic base and PDMS piece pass through glue interlayer adhesion into an entirety, connect conduit in the punching of PDMS on piece, being passed through microfluid can come into operation.Crystalline ceramics micro-fluidic chip produced by the present invention can height Bionics Bone environment, it can be realized high-flux medicaments sifting, the present invention has innovatively used hydroxyapatite as the material of micro-fluidic chip, and the good biocompatibility of hydroxyapatite is conducive to cell in chip surface tactophily.The transparence that material is realized by the high temperature high-pressure sinter mode such as hot isostatic pressing, meets the optical characteristics demand of micro-fluidic chip.Ceramic surface is covered with PDMS piece, ensure that cell can on chip long-term cultivation.
Description
Technical field
The present invention relates to the technical fields of crystalline ceramics preparation and micro-fluidic chip, refer in particular to a kind of crystalline ceramics miniflow
Control the preparation method of chip.
Background technique
Traditional micro-fluid chip material cannot analog bone microenvironment well.Initial micro-fluidic technologies are in silicon wafer
Or microchannel structure is constructed using optical etching technology on glass, it is time-consuming and laborious.Dimethyl silicone polymer (PDMS's) mentions
The high efficiency of micro-fluidic technologies simultaneously greatly reduces cost, but PDMS also has its limitation as bone object official chip.PDMS has
When can absorb or leach nonpolarity or low pole small molecule, and it is incompatible with organic solvent, needed before sowing cell into
The cumbersome surface modification of row.Most of all, PDMS component and the calcium phosphate component in bone are entirely different.Hydroxyapatite
(HAP) be human body and animal skeleton main inorganic composition, can participate in vivo be metabolized, have bioactivity, be as bone object official
The ideal material of the bionical human body bone microenvironment of chip.Photocuring ceramics 3D printing technique have formed precision is high, structure is complicated, one
The advantages of secondary molding, solves the problems, such as the processing of ceramic material brittleness disaster；Personalizable design is to prepare the micro-fluidic core of ceramics
The ideal chose of piece.
Summary of the invention
The purpose of the present invention is to overcome the shortcomings of the existing technology and deficiency, proposes a kind of crystalline ceramics micro-fluidic chip
Preparation method, crystalline ceramics micro-fluidic chip obtained can height Bionics Bone environment, can be realized high-flux medicaments sifting, lead to
Cross the material that this method has innovatively used hydroxyapatite as micro-fluidic chip, the good bio-compatible of hydroxyapatite
Property is conducive to cell in chip surface tactophily.The transparent of material is realized by the high temperature high-pressure sinter mode such as hot isostatic pressing
Change, meets the optical characteristics demand of micro-fluidic chip.Ceramic surface is covered with a strata dimethyl siloxane cover board (hereinafter referred to as
PDMS piece), the good oxygen transmission rate of PDMS piece ensure that cell can on chip long-term cultivation.
To achieve the above object, a kind of technical solution provided by the present invention are as follows: preparation of crystalline ceramics micro-fluidic chip
Method, comprising the following steps:
1) base part of micro-fluidic chip is designed in modeling software, substrate surface has very low power pattern, by institute
The substrate of design exports as stl model；
2) the substrate model that step 1) obtains is imported into photocuring ceramic printer, prints skill using photocuring ceramics
Art successively prints, one-step shaping, and used printed material is hydroxyapatite, and the ceramic bases for obtaining micro-fluidic chip are raw
Base；
3) by the ceramic bases green compact that step 2) obtains be put into high temperature furnace slowly it is degreasing sintered, then pass through high temperature and pressure
Sintering, obtains transparent ceramic bases；
4) dimethoxysiloxane host agent and curing agent are uniformly mixed with mass ratio 10:1 ratio, obtain mixed liquor, benefit
Make the bubble in mixed liquor floating to surface with the mode vacuumized and rupture, places into baking oven a period of time that is heating and curing, obtain
To dimethyl silicone polymer cover board, referred to as PDMS piece；
5) according to transparent ceramic bases shape and very low power pattern, the obtained PDMS piece of step 4) is cut,
And punched in corresponding position, punching diameter is consistent with external catheter outer diameter is needed, the PDMS piece having been had openning hole；
6) the PDMS piece for obtaining step 5) is Nian Jie by glue with the transparent ceramic base that step 3) obtains, and reheats solid
Change, target product can be obtained, crystalline ceramics micro-fluidic chip completes.
Further, the crystalline ceramics micro-fluidic chip that step 6) obtains is plugged into external conduit, conduit is passed through microfluid,
Crystalline ceramics micro-fluidic chip just can come into operation.
Further, the production method of the ceramic bases green compact uses stereolithography apparatus (Stereo
Lithography Appearance, SLA) or digital light processing (Digital Light Processing, DLP).
Further, the method that the ceramic bases bleach uses is hot isostatic pressing method, atmosphere and vaccum sintering process, electric discharge
One of plasma sintering method or several combinations.
Further, the material of the conduit is one or more of PTFE, PE, PEEK combination.
Further, the outer diameter of the conduit is 0.5mm~2mm.
Further, the glue is the liquid dimethyl radical siloxane that diluted of methylene chloride, dilution ratio is 30%~
100%.
Further, in step 4), the solidification temperature of the PDMS piece is 65 DEG C~85 DEG C, and curing time is 1h~4h.
Compared with prior art, the present invention have the following advantages that with the utility model has the advantages that
A kind of crystalline ceramics micro-fluidic chip of height Bionics Bone microenvironment can be obtained by the method for the invention, had resistance to
High temperature, acid-alkali-corrosive-resisting, it is wear-resistant the advantages that, no longer need to carry out cumbersome surface modification before sowing cell, can be used for
It realizes high-flux medicaments sifting, and probes into osteocyte and the interaction of other cells etc., there is biggish actual promotional value.
Detailed description of the invention
Fig. 1 is the underlying structure schematic diagram of ceramic micro-fluidic chip.
Fig. 2 is the exploded view of crystalline ceramics micro-fluidic chip.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1
The first step draws an Xmas-tree micro-fluidic chip using rhino software, and channel width is 200 μm, channel height
It is 200 μm, totally four groups of parallel channels, export stl model file.Second step is printed model using DLP ceramic printer
Coming, used printed material is hydroxyapatite, obtains the ceramic bases green compact of micro-fluidic chip, it is shown in Figure 1, in figure
1 is substrate, and 2 be the very low power pattern in substrate.The ceramic bases green compact printed are put in degreasing in high temperature furnace and burnt by third step
Knot, keeps the temperature 1h by 1280 degree of maximum temperature.Afterwards by ceramic bases put into hot isostatic pressure stove (it is of course also possible to select atmosphere with
Vaccum sintering process or discharge plasma sintering process, several combinations being also possible in them), 3 DEG C/min, 1200 DEG C of heat preservations
5h obtains transparent ceramic bases.4th step mixes dimethoxysiloxane host agent and curing agent with mass ratio 10:1 ratio
Uniformly, after vacuumizing 20min, 65 DEG C of solidification 4h obtain dimethyl silicone polymer cover board (referred to as PDMS piece), referring to fig. 2 institute
Show, 3 be PDMS piece in figure.PDMS piece is cut into size consistent with ceramic bases, is punched by the 5th step, and punching diameter is
1mm.The liquid dimethyl siloxane of 10:1 is diluted to 30% using methylene chloride, is applied to PDMS on piece by the 6th step, and saturating
Bright ceramic bases are pasted together, and are put into baking oven, 75 DEG C of solidification 2h.7th step, being inserted into three outer diameters is 0.5mm~2mm (In
The preferred 1mm of the present embodiment) conduit (can be one or more of PTFE, PE, PEEK combination), it is shown in Figure 2, in figure
4 be conduit, and facture of microchip is completed.8th step, verifying: micro-fluidic chip is passed through cell suspending liquid, cell density 100
Ten thousand/milliliter after culture one day, are passed through cell dead fluorescent dye living and are placed under fluorescence microscope and see after dyeing half an hour
It examines, cell state is good, and living cells quantity meets cell culture far more than dead cell quantity, Xmas-tree ceramics micro-fluidic chip
Requirement.
Embodiment 2
The first step draws an Xmas-tree micro-fluidic chip using solidworks software, and channel width is 100 μm, is led to
Road height is 100 μm, totally eight groups of parallel channels, exports stl model file.Second step is played model using SLA ceramic printer
It prints off and, used printed material is hydroxyapatite, obtains the ceramic bases green compact of micro-fluidic chip.Third step will be beaten
The substrate green compact printed off be put in it is degreasing sintered in high temperature furnace, 1280 degree of maximum temperature, keep the temperature 1h.Put ceramic bases into heat etc. afterwards
Static pressure sintering furnace (it is of course also possible to select atmosphere and vaccum sintering process or discharge plasma sintering process, is also possible to them and works as
In several combinations), 5 DEG C/min, 1200 DEG C of heat preservation 3h obtain transparent ceramic bases.4th step, by dimethoxysiloxane
Host agent and curing agent are uniformly mixed with mass ratio 10:1 ratio, and after vacuumizing 20min, 85 DEG C of solidification 1h obtain poly dimethyl silicon
Oxygen alkane cover board (referred to as PDMS piece).PDMS piece is cut into size consistent with ceramic bases, is punched by the 5th step, punching
Diameter is 1.4mm.The liquid dimethyl siloxane of 10:1 is diluted to 100% using methylene chloride, is applied to pdms by the 6th step
On piece is pasted together with transparent ceramic bases, is put into baking oven, 80 DEG C of solidification 1h.7th step, being inserted into three outer diameters is
The conduit (can be one or more of PTFE, PE, PEEK combination) of 0.5mm~2mm (in the preferred 1.4mm of the present embodiment),
Facture of microchip is completed.8th step, verifying: the external conduit in micro-fluidic chip two sides each leads into red glimmering with green
Light ink is placed under laser confocal microscope and observes, and measures the fluorescence intensity of each parallel channels, shows good
Gradient distribution rule.
Embodiment described above is only the preferred embodiments of the invention, and but not intended to limit the scope of the present invention, therefore
All shapes according to the present invention change made by principle, should all be included within the scope of protection of the present invention.
Claims (8)
1. a kind of preparation method of crystalline ceramics micro-fluidic chip, which comprises the following steps:
1) base part of micro-fluidic chip is designed in modeling software, substrate surface has very low power pattern, will be designed
Substrate export as stl model；
2) the substrate model that step 1) obtains is imported into photocuring ceramic printer, using photocuring ceramics printing technique,
Successively printing, one-step shaping, used printed material are hydroxyapatite, obtain the ceramic bases green compact of micro-fluidic chip；
3) by the ceramic bases green compact that step 2) obtains be put into high temperature furnace slowly it is degreasing sintered, then by high temperature and pressure burning
Knot, obtains transparent ceramic bases；
4) dimethoxysiloxane host agent and curing agent are uniformly mixed with mass ratio 10:1 ratio, obtain mixed liquor, utilizes pumping
The mode of vacuum makes the bubble in mixed liquor floating to surface and ruptures, and places into baking oven a period of time that is heating and curing, is gathered
Dimethyl siloxane cover board, referred to as PDMS piece；
5) according to transparent ceramic bases shape and very low power pattern, the obtained PDMS piece of step 4) is cut, and
Corresponding position punching, punching diameter is consistent with external catheter outer diameter is needed, the PDMS piece having been had openning hole；
6) the PDMS piece for obtaining step 5) is Nian Jie by glue with the transparent ceramic base that step 3) obtains, and reheats solidification,
Target product can be obtained, crystalline ceramics micro-fluidic chip completes.
2. a kind of preparation method of crystalline ceramics micro-fluidic chip according to claim 1, it is characterised in that: by step 6)
Obtained crystalline ceramics micro-fluidic chip plugs external conduit, and conduit is passed through microfluid, and crystalline ceramics micro-fluidic chip just can
Enough come into operation.
3. a kind of preparation method of crystalline ceramics micro-fluidic chip according to claim 1, it is characterised in that: the ceramics
The production method of substrate green compact is using stereolithography apparatus or digital light processing.
4. a kind of preparation method of crystalline ceramics micro-fluidic chip according to claim 1, it is characterised in that: the ceramics
The method that substrate bleach uses is one of hot isostatic pressing method, atmosphere and vaccum sintering process, discharge plasma sintering process
Or several combinations.
5. a kind of preparation method of crystalline ceramics micro-fluidic chip according to claim 1, it is characterised in that: the conduit
Material be one or more of PTFE, PE, PEEK combination.
6. a kind of preparation method of crystalline ceramics micro-fluidic chip according to claim 1, it is characterised in that: the conduit
Outer diameter be 0.5mm~2mm.
7. a kind of preparation method of crystalline ceramics micro-fluidic chip according to claim 1, it is characterised in that: the glue
For the liquid dimethyl radical siloxane that methylene chloride diluted, dilution ratio is 30%~100%.
8. a kind of preparation method of crystalline ceramics micro-fluidic chip according to claim 1, it is characterised in that: in step 4)
In, the solidification temperature of the PDMS piece is 65 DEG C~85 DEG C, and curing time is 1h~4h.
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Cited By (7)
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| CN111589477A (en) * | 2020-05-28 | 2020-08-28 | 韶关学院 | Micro-channel device processing technology |
| CN111685755A (en) * | 2020-05-29 | 2020-09-22 | 华南理工大学 | AgNWs-PDMS composite flexible conductive optical fiber micro-lens and preparation method thereof |
| CN113368915A (en) * | 2021-06-28 | 2021-09-10 | 上海交通大学 | Micro-fluidic chip for high-flux culture of brain organoids |
| CN115055137A (en) * | 2022-08-04 | 2022-09-16 | 之江实验室 | Processing method of microreactor |
| CN115106034A (en) * | 2022-06-23 | 2022-09-27 | 之江实验室 | Visual microreactor and preparation method thereof |
| CN115193498A (en) * | 2022-07-26 | 2022-10-18 | 之江实验室 | Ceramic micro-fluidic chip and preparation method and application thereof |
| CN115304376A (en) * | 2022-08-09 | 2022-11-08 | 之江实验室 | Transparent ceramic micro-fluidic chip and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111589477A (en) * | 2020-05-28 | 2020-08-28 | 韶关学院 | Micro-channel device processing technology |
| CN111685755A (en) * | 2020-05-29 | 2020-09-22 | 华南理工大学 | AgNWs-PDMS composite flexible conductive optical fiber micro-lens and preparation method thereof |
| CN111685755B (en) * | 2020-05-29 | 2021-09-21 | 华南理工大学 | AgNWs-PDMS composite flexible conductive optical fiber micro-lens and preparation method thereof |
| CN113368915A (en) * | 2021-06-28 | 2021-09-10 | 上海交通大学 | Micro-fluidic chip for high-flux culture of brain organoids |
| CN115106034A (en) * | 2022-06-23 | 2022-09-27 | 之江实验室 | Visual microreactor and preparation method thereof |
| CN115106034B (en) * | 2022-06-23 | 2024-06-11 | 之江实验室 | Visual micro-reactor and preparation method thereof |
| CN115193498A (en) * | 2022-07-26 | 2022-10-18 | 之江实验室 | Ceramic micro-fluidic chip and preparation method and application thereof |
| CN115193498B (en) * | 2022-07-26 | 2024-04-16 | 之江实验室 | Ceramic micro-fluidic chip and preparation method and application thereof |
| CN115055137A (en) * | 2022-08-04 | 2022-09-16 | 之江实验室 | Processing method of microreactor |
| CN115055137B (en) * | 2022-08-04 | 2024-02-06 | 之江实验室 | Processing method of microreactor |
| CN115304376A (en) * | 2022-08-09 | 2022-11-08 | 之江实验室 | Transparent ceramic micro-fluidic chip and preparation method thereof |
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