CN107474225B - A kind of method that chemical vapour deposition technique prepares Parylene nanofiber - Google Patents
A kind of method that chemical vapour deposition technique prepares Parylene nanofiber Download PDFInfo
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- CN107474225B CN107474225B CN201710855165.0A CN201710855165A CN107474225B CN 107474225 B CN107474225 B CN 107474225B CN 201710855165 A CN201710855165 A CN 201710855165A CN 107474225 B CN107474225 B CN 107474225B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G61/02—Macromolecular compounds containing only carbon atoms in the main chain of the macromolecule, e.g. polyxylylenes
- C08G61/025—Polyxylylenes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/76—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from other polycondensation products
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/10—Definition of the polymer structure
- C08G2261/11—Homopolymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/10—Definition of the polymer structure
- C08G2261/14—Side-groups
- C08G2261/141—Side-chains having aliphatic units
- C08G2261/1414—Unsaturated aliphatic units
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/10—Definition of the polymer structure
- C08G2261/14—Side-groups
- C08G2261/142—Side-chains containing oxygen
- C08G2261/1422—Side-chains containing oxygen containing OH groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
- C08G2261/34—Monomer units or repeat units incorporating structural elements in the main chain incorporating partially-aromatic structural elements in the main chain
- C08G2261/342—Monomer units or repeat units incorporating structural elements in the main chain incorporating partially-aromatic structural elements in the main chain containing only carbon atoms
- C08G2261/3424—Monomer units or repeat units incorporating structural elements in the main chain incorporating partially-aromatic structural elements in the main chain containing only carbon atoms non-conjugated, e.g. paracyclophanes or xylenes
Abstract
The invention discloses a kind of methods that chemical vapour deposition technique prepares Parylene nanofiber, belong to field of material technology.The present invention uses chemical vapour deposition technique, using Parylene as presoma, using nematic crystal as template, Parylene nanofiber is successfully prepared by vapor deposition polymerization reaction, the preparation method has the characteristics that the size of fiber itself, pattern, composition are controllable, avoid conventional electrostatic spin processes prepare fiber there are problems that solvent post-processing, the disadvantages of environmental pollution is serious, gained can be applied to drug delivery system, organizational project, microfluidic device etc., have very high application value.
Description
Technical field
The invention belongs to field of material technology, are related to the preparation of polymer nanofiber, and in particular to a kind of chemical gaseous phase
The method that sedimentation prepares Parylene nanofiber.
Background technique
In recent years, polymer nanofiber is with unique advantages such as the specific surface area of its superelevation, good flexible and ductility,
In various fields such as nano-sensor, tissue engineering bracket, filter medium, drug delivery, artificial blood vessel, biochip, military
Protective garment, optics and composite material etc. show extremely strong vitality, and become grinding for the fields such as high molecular material, biological medicine
Study carefully hot spot.Currently, the research hotspot of polymer nanofiber is concentrated mainly on field of biomedicine, may be used as functional membrane,
Cytoskeleton, biomimetic material, cell carrier etc..
The preparation method of common nanofiber mainly has pulling method, templated synthesis, microphase-separated, self assembly and Static Spinning
Silk etc..Wherein, method of electrostatic spinning have many advantages, such as it is easy to operate, have a wide range of application and be widely used.This method is prepared
Fiber there is lot of advantages, such as biggish specific surface area, higher porosity, aperture have a very wide distribution, morphosis
Also the features such as similar with natural cytoplasm.However, method of electrostatic spinning is mainly for solvent spinning system, production efficiency compared with
It is low, and volume production problem needs to solve.Melting electrostatic spinning method is not limited by solvent, but due to the high viscosity of molten polymer,
The fibre diameter that this method is prepared is difficult to be less than 500nm, and there is also certain disadvantages for some other method.Currently, Nanowire
Dimension type is limited, fiber functional modification technology is still immature.Therefore, develop synthetic polymer nanofiber new technology with
And to it carry out functional modification is the developing direction of polymer nanofiber.
Parylene (PPX) is a kind of unbranched, highly crystalline, the heat with unique poly- two methylenes penylene structure
Plastic macromolecule material.It has it is high-purity, fine and close, have extremely good electrical insulating property, heat resistance, weatherability and chemical stabilization
Property.Parylene generally as conformal coat material, uniform coating thickness is controllable, it is fine and close it is pin-free, transparent it is unstressed, without helping
The advantages that agent, is mainly prepared using chemical vapor deposition polymerization (CVD) method at present.However, Parylene is insoluble in many
Solvent cannot act as the coating based on solvent, film or fiber can not be formed it into solution, at present in industry
On application receive the obstruction of traditional manufacturing technology.Therefore, searching exploitation is novel, is simple and efficient, environmental-friendly Nanowire
It is very necessary to tie up technology of preparing.
Summary of the invention
It is lower in order to solve production efficiency existing for traditional fibre manufacturing technology, and there are solvent post-processings, environmental pollution
The problem of, the present invention provides it is a kind of simple, efficiently, method that polymer nanofiber is prepared under temperate condition, this method gram
The solvent post-processing problem of traditional fibre preparation method is taken, and invention reaction condition is simple, reaction process is mildly rapid, and shape
Looks are controllable.
To achieve the above objectives, the present invention is to adopt the following technical scheme that be achieved:
A kind of method that chemical vapour deposition technique prepares Parylene nanofiber, comprising the following steps:
Using paraxylene dimer or derivatives thereof as presoma, it is placed in CVD sublimation zone, nematic crystal is placed in band
Have on the micro slide of copper mesh, and places it on settling chamber's sample stage；
500~550 DEG C of chamber target temperature of setting cracking, while system being maintained under relatively low vacuum degree, to heavy
After product area's temperature reaches set temperature, vacuum degree is improved, when reaching 0.08Torr or more, in deposition rateUnder,
Start to carry out CVD polymerization, the temperature of sample stage is -10~20 DEG C；
CVD removes remaining liquid crystal after reaction, by the micro slide soaked in solvent for having CVD coating, after natural drying
Obtain Parylene nanofiber.
The nematic crystal is E7, TL205 or 5CB.
The presoma is paraxylene dimer, 4- methylol-paraxylene dimer and 4- acetenyl-to diformazan
One or more of benzene dimer.
The solvent selects dehydrated alcohol, acetone or hexane, preferably dehydrated alcohol.
The cracking temperature is 530 DEG C, -10 DEG C of sample stage temperature, deposition rate
The micro slide is silicon substrate micro slide, auri body micro slide or sheet glass, preferably sheet glass.
The micro slide and copper mesh removes its surface impurity, then will cleaning before use, be first ultrasonically treated with dehydrated alcohol
Clean micro slide is spare after being handled with silane coupling reagent.
Compared with prior art, the present invention has the following technical effects and advantage:
The present invention prepares Parylene nanofiber using CVD method in liquid crystal template, it is desirable to provide a kind of polymer
The controllable method for preparing of nanofiber, this method mainly pass through chemical vapour deposition technique, and the advantages of combination template, with nematic
Type thermotropic liquid crystal is template, prepares parylene polymer nanofiber using CVD method；The presoma of CVD method passes through cracking
The cracking in area, mixing free radical enter sample stage, and gap of the living radical after CVD is cracked between liquid crystal molecule is raw
It is long；Some by-products adjoint in liquid phase reactor, harmful chemical reagent, solvent, catalyst, initiator etc. can effectively be avoided.
The solvent post-processing problem of traditional fibre preparation method being overcome, and invention reaction condition is simple, reaction process is mildly rapid, and
Morphology controllable.Therefore, polymer nanofiber prepared by the present invention can be widely applied to technical field of fiber preparation, and open up
Open up application of the Parylene in field of biomedicine such as organizational project, biomedical devices.The preparation method has fiber
The controllable feature of itself size, pattern, composition avoids conventional electrostatic spin processes and prepares fiber there are solvent post-processings to ask
The disadvantages of topic, environmental pollution is serious, gained can be applied to drug delivery system, organizational project, microfluidic device etc., have very high
Application value.
Detailed description of the invention
Fig. 1 is the specific flow chart that the present invention is implemented.
Fig. 2 is Fourier's infrared spectrum (FT- of the resulting Parylene nanofiber of institute's embodiment 2 and 3 of the present invention
IR) spectrogram.
Fig. 3 is the SEM photograph of Parylene nanofiber, a) PPX-N nanofiber；b)PPX-CH2OH nanofiber.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
A kind of method that chemical vapour deposition technique prepares Parylene nanofiber, the steps include: with paraxylene two
Aggressiveness or derivatives thereof (having different functional groups) is presoma, is put into the sublimation zone of CVD device.Nematic crystal is placed in band
Have on the sheet glass of copper mesh, and take liquid crystal on copper mesh with micro syringe, ready sheet glass is placed on settling chamber's sample
In sample platform.The temperature of cracking chamber is set to target temperature, while system being maintained under relatively low vacuum degree, CVD is started
Polymerization.Presoma mixes free radical and enters sample stage, the living radical after CVD is cracked is along liquid by the cracking of cracking zone
Void growth between brilliant molecule.CVD removes remaining liquid after reaction, by the sheet glass soaked in solvent for having CVD coating
Nanofiber can be obtained after natural drying in crystalline substance.The preparation flow of nanofiber is as shown in Figure 1.
Wherein, CVD cracking temperature is 500~550 DEG C, and sample stage temperature is -10~20 DEG C.Deposition rateComprehensively considering the pattern and its performance of Parylene nanofiber, preferably cracking temperature is preferably 530 DEG C,
- 10 DEG C of sample stage temperature, deposition rate
It is right that polymer precursor can be paraxylene dimer, 4- methylol-paraxylene dimer and 4- acetenyl-
One or more of dimethylbenzene dimer.The nematic crystal is E7, TL205 or 5CB.Such as silicon and gold on any matrix
Nanofiber can be obtained on matrix, sheet glass mainly useful for is selected to observe under the microscope.CVD after reaction, is selected
Dehydrated alcohol, acetone, hexane equal solvent, wherein preferred dehydrated alcohol.
Embodiment 1
The preparation of Parylene nanofiber: sheet glass and copper mesh are ultrasonically treated with dehydrated alcohol, remove its surface
Impurity.Again by the sheet glass cleaned up with silane coupling reagent handle a period of time after it is spare.Nematic crystal is placed in band
Have on the sheet glass of copper mesh, and takes 7 μ l liquid crystal on copper mesh with 10 μ l micro syringes.It is heavy that ready sheet glass is placed on
On product room sample stage.The presoma of CVD reaction is 10g paraxylene dimer.The temperature for cracking chamber is risen into target temperature 530
DEG C, while system being maintained under relatively low vacuum degree, after area's temperature to be deposited reaches set temperature, vacuum degree is improved,
When reaching 0.08Torr, CVD polymerization is carried out under certain deposition rate.Living radical after CVD is cracked is along liquid crystal point
Void growth between son.After CVD, there will be the sheet glass of CVD coating to be soaked for a period of time with ethanol solution, removes
Nanofiber can be obtained after natural drying in remaining liquid crystal on sheet glass.
Embodiment 2
The preparation (other steps are same as Example 1) of Parylene nanofiber: 10g paraxylene dimer is set
In CVD sublimation zone, 550 DEG C of cracking temperature, deposition rate isSample stage temperature is 0 DEG C.On nematic crystal E7
Carry out CVD polymerization.After soaked in absolute ethyl alcohol, nanofiber is obtained after drying.
Embodiment 3
The preparation (other steps are same as Example 1) of Parylene nanofiber: by the 4- methylol-of 10g to two
Toluene dimer is placed in CVD sublimation zone, and 500 DEG C of cracking temperature, deposition rate isSample stage temperature is -10 DEG C.?
CVD polymerization is carried out on nematic crystal E7.After being impregnated with hexane, nanofiber is obtained after drying.
As shown in Fig. 2, a and b respectively represent PPX-N nanofiber and PPX-CH2OH nanofiber.It can from figure
Out, PPX-N nanofiber is in 3100cm-1Left and right and 1650~1450cm-1Between appearance, this is the characteristic absorption of PPX phenyl ring
Peak.2922cm-1And 2855cm-1Place is the stretching vibration absworption peak of methylene, and PPX-CH2The infrared signature peak of OH nanofiber
In other than the characteristic peak containing PPX-N, in 3350cm-1There is-OH characteristic absorption peak in place, this shows can using CVD method
To obtain Parylene nanofiber in liquid crystal matrix.
Fig. 3 is the SEM photograph of Parylene nanofiber prepared by the present invention, a) PPX-N nanofiber；b)PPX-
CH2OH nanofiber.It can be seen that the Parylene of different functional groups can obtain polymer nanocomposite in liquid crystal matrix
Fiber.Fiber morphology is regular, is evenly distributed, and is in align.
Embodiment 4
The preparation (other steps are same as Example 1) of Parylene nanofiber: by the paraxylene dimer of 10g
It is placed in CVD sublimation zone, 550 DEG C of cracking temperature, deposition rate isSample stage temperature is -10 DEG C.In nematic crystal
CVD polymerization is carried out on TL205.After soaked in absolute ethyl alcohol, nanofiber is obtained after drying.
Embodiment 5
The preparation (other steps are same as Example 1) of Parylene nanofiber: by the 4- acetenyl-of 10g to two
Toluene dimer is placed in CVD sublimation zone, and 530 DEG C of cracking temperature, deposition rate isSample stage temperature is 10 DEG C.?
CVD polymerization is carried out on nematic crystal E7.After soaked in absolute ethyl alcohol, nanofiber is obtained after drying.
Embodiment 6
The preparation (other steps are same as Example 1) of Parylene nanofiber: by the 4- acetenyl-of 10g to two
Toluene dimer is placed in CVD sublimation zone, and 530 DEG C of cracking temperature, deposition rate isSample stage temperature is -10 DEG C.?
CVD polymerization is carried out on nematic crystal 5CB.After acetone soak, nanofiber is obtained after drying.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of method that chemical vapour deposition technique prepares Parylene nanofiber, which comprises the following steps:
Using paraxylene dimer or derivatives thereof as presoma, it is placed in CVD sublimation zone, nematic crystal is placed in copper
On the micro slide of net, and place it on settling chamber's sample stage；
500~550 DEG C of chamber target temperature of setting cracking, while system being maintained under relatively low vacuum degree, area to be deposited
After temperature reaches set temperature, vacuum degree is improved, when reaching 0.08Torr or more, in deposition rateUnder, start
CVD polymerization is carried out, the temperature of sample stage is -10~20 DEG C；
CVD removes remaining liquid crystal after reaction, by the micro slide soaked in solvent for having CVD coating, obtains after natural drying
Parylene nanofiber.
2. the method that chemical vapour deposition technique according to claim 1 prepares Parylene nanofiber, feature exist
In: the nematic crystal is E7, TL205 or 5CB.
3. the method that chemical vapour deposition technique according to claim 1 prepares Parylene nanofiber, feature exist
In: the presoma is paraxylene dimer, 4- methylol-paraxylene dimer and 4- acetenyl-paraxylene two
One or more of aggressiveness.
4. the method that chemical vapour deposition technique according to claim 1 prepares Parylene nanofiber, feature exist
In: the solvent selects dehydrated alcohol, acetone or hexane.
5. the method that chemical vapour deposition technique according to claim 1 or 4 prepares Parylene nanofiber, feature
Be: the solvent selects dehydrated alcohol.
6. the method that chemical vapour deposition technique according to claim 1 prepares Parylene nanofiber, feature exist
In: the cracking temperature is 530 DEG C, -10 DEG C of sample stage temperature, deposition rate
7. the method that chemical vapour deposition technique according to claim 1 prepares Parylene nanofiber, feature exist
In: the micro slide is silicon substrate micro slide, auri body micro slide or sheet glass.
8. the method that chemical vapour deposition technique according to claim 1 or claim 7 prepares Parylene nanofiber, feature
Be: the micro slide is sheet glass.
9. the method that chemical vapour deposition technique according to claim 1 prepares Parylene nanofiber, feature exist
In: the micro slide and copper mesh before use, being first ultrasonically treated with dehydrated alcohol, its surface impurity is removed, then will clean up
Micro slide handled with silane coupling reagent after it is spare.
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| US10450677B2 (en) | 2018-01-18 | 2019-10-22 | California Institute Of Technology | Method to manufacture microfibers and microcapillaries |
| CN108505129A (en) * | 2018-04-09 | 2018-09-07 | 南京捷纳思新材料有限公司 | A kind of device for spinning and technique preparing ordered nano-fibers array |
| KR102593110B1 (en) * | 2021-09-29 | 2023-10-25 | 충남대학교산학협력단 | Novel polymer and method for forming patterns using the same |
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| US6586048B2 (en) * | 2001-04-05 | 2003-07-01 | Honeywell International Inc. | Method for depositing a barrier coating on a polymeric substrate and composition comprising said barrier coating |
| CN1915807A (en) * | 2006-09-07 | 2007-02-21 | 上海交通大学 | Method for preparing Nano carbon fiber |
| CN105420689B (en) * | 2015-11-06 | 2019-06-07 | 中国人民解放军国防科学技术大学 | A kind of aligned carbon nanotube-aluminum oxide hybridization fiber and preparation method thereof |
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