CN109256239A - Poly- (3- hexyl thiophene) conductive network structure of one kind and preparation method thereof - Google Patents
Poly- (3- hexyl thiophene) conductive network structure of one kind and preparation method thereof Download PDFInfo
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- CN109256239A CN109256239A CN201810848629.XA CN201810848629A CN109256239A CN 109256239 A CN109256239 A CN 109256239A CN 201810848629 A CN201810848629 A CN 201810848629A CN 109256239 A CN109256239 A CN 109256239A
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- hexyl thiophene
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
- H01B1/124—Intrinsically conductive polymers
- H01B1/127—Intrinsically conductive polymers comprising five-membered aromatic rings in the main chain, e.g. polypyrroles, polythiophenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
Abstract
The invention discloses a kind of poly- (3- hexyl thiophene) conductive network structures and preparation method thereof.This method prepares super high molecular polyethylene solution, ultra-high molecular weight polyethylene shish-kebab network structure will be prepared on the solution spin coating hot silicon wafer after oxidation by spin coating instrument；Then poly- (3- hexyl thiophene) conductive network structure is prepared in poly- (3- hexyl thiophene) the solution drop coating of preparation in above-mentioned network structure.This method is simply easily operated, and preparation time is short, high-efficient；Obtained network structure is circlewise regularly arranged, and there is good electric conductivity to have a good application prospect as conducting polymer network.
Description
Technical field
The invention belongs to conducting polymer processing technique fields.More particularly to a kind of poly- (3- hexyl thiophene) conductive network knot
Structure and preparation method thereof.
Technical background
The discovery of conducting polymer has extremely important influence for microelectronics, the innovation of optoelectronics industry manufacturing technology.It leads
Not only there is electric polymer unique electric (light, magnetic) to learn property, but also easy to process, have unique combining properties, this is it
Not available for his material.
Poly- (3- hexyl thiophene) (abbreviation P3HT) has unique structure feature as a kind of excellent conjugate photoelectric material
(pi-electron conjugated system), because its is at low cost, field effect mobility is high, and solution processability is strong, and compared to other polythiophene materials
Material has higher self-organizing and charge transport properties, show that it in light, field effect transistor and in terms of,
With very big potential application market.Therefore, since self-discovery conducting polymer, which is received significant attention, and has carried out depth
The exploratory development entered.Currently, there are mainly three types of the methods for inducing poly- (3- hexyl thiophene) to crystallize, first, in one layer of oriented film
On with the method for melt membrane induce poly- (3- hexyl thiophene) crystallization, due to poly- (3- hexyl thiophene) in the process without and silicon wafer
It directly contacts, conductive effect is very poor；Second, using solvent evaporated method, but process is slow, inefficient, and operation difficulty is big；Its
Three, poly- (3- hexyl thiophene) epitaxial crystallization is induced using other high molecular polymers, but each poly- (3- hexyl thiophene) crystal
Between lack connection, and cause its electric conductivity poor.
Polyethylene possesses succinct chemical structure as a kind of typical semicrystalline polymeric.Superhigh molecular weight polyethylene
Alkene is a kind of thermoplastic engineering plastic with excellent comprehensive performance of linear structure, and super high molecular polyethylene solution passes through super
High drawing process will form shish-kebab network structure, and extended-chain crystal is used as " shish " in this structure, folded-chain crystal
As " kebab ", therefore, which has good thermal stability, can preferably be used as poly- (3- hexyl thiophene) conductive mesh
The inductor of network structure preparation.
The present invention is easy the performance being nucleated on other materials surface using poly- (3- hexyl thiophene), by poly- (3- hexyl thiophene
Pheno) it is combined with ultra-high molecular weight polyethylene, poly- (3- hexyl thiophene) epitaxial crystallization system is induced using ultra-high molecular weight polyethylene
It is standby to have obtained poly- (3- hexyl thiophene) conductive network.
Summary of the invention
To achieve the goals above, the present invention provides a kind of poly- (3- hexyl thiophene) conductive network structure and its preparation sides
Method, this method is simply easily operated, the time is short, high-efficient, and poly- (3- hexyl thiophene) the conductive network structure being prepared has
Good electric conductivity；
In addition, poly- (3- hexyl thiophene) the conductive network structure being prepared by this method, P3HT nanofiber (P3HT
Crystal) it is microcosmic on take edge-on to be orientated, uniformly and be arranged vertically in ultra-high molecular weight polyethylene network structure, form
Shish-kebab structure, and be macroscopically isotropic, and by ultra-high molecular weight polyethylene network structure, each
P3HT crystal connects each other and forms network structure；The P3HT nanofiber (P3HT crystal) and silicon wafer being prepared directly connect
Touching, above structure enhance network structure electric conductivity.
The present invention is achieved by the following technical solutions
A kind of preparation method of poly- (3- hexyl thiophene) conductive network structure, method includes the following steps:
(1) preparation of ultra-high molecular weight polyethylene shish-kebab network structure:
A. it takes ultra-high molecular weight polyethylene to carry out dissolution mixing in a solvent, then mixture is heated, surpassed
High molecular weight polyethylene solution；
B. silicon wafer is taken, oxidation processes are carried out to silicon wafer, after the completion of oxidation processes, the silicon wafer after oxidation is placed in spin coating instrument
In, then the silicon wafer being placed on spin coating instrument is heated and kept the temperature；
C. super after being dissolved by heating described in step a rapidly after the completion of the silicon wafer heating and thermal insulation on spin coating instrument described in step b
High molecular weight polyethylene solution, which is placed on the silicon wafer of spin coating instrument, carries out spin coating, after the completion of spin coating, the superelevation that will be spin-coated on silicon wafer
Molecular weight polyethylene is cooled to room temperature to arrive ultra-high molecular weight polyethylene shish-kebab network structure；
(2) (ultra-high molecular weight polyethylene induces poly- (3- hexyl thiophene for the preparation of poly- (3- hexyl thiophene) conductive network structure
Pheno) epitaxial crystallization prepares conductive network structure):
D. it takes poly- (3- hexyl thiophene) to be dissolved in solvent, then the mixed solution of poly- (3- hexyl thiophene) and solvent is carried out
Heating is completely dissolved poly- (3- hexyl thiophene), and poly- (3- hexyl thiophene) solution is obtained after being completely dissolved；
E. the super high molecular weight poly- (3- hexyl thiophene) the solution drop coating that step d is obtained being prepared in step (1) is poly-
In ethylene shish-kebab network structure；It after the completion of drop coating, volatilizees naturally, solvent obtains poly- (3- hexyl thiophene after volatilizing completely
Pheno) conductive network structure；
Or the ultra-high molecular weight polyethylene shish- being cooled to room temperature on the silicon wafer that step (1) is prepared first
Kebab network structure is heated, and it is identical as poly- (3- hexyl thiophene) temperature of solution obtained by step d to be heated to temperature, heating
After the completion, it keeps the temperature at such a temperature；After the completion of heat preservation, then by poly- (3- hexyl thiophene) solution drop coating obtained by step d after heat preservation
In ultra-high molecular weight polyethylene shish-kebab network structure on silicon wafer；It after the completion of drop coating, volatilizees naturally, solvent is waved completely
The conductive network structure of poly- (3- hexyl thiophene) is obtained after hair.
Further, the solvent that ultra-high molecular weight polyethylene is dissolved described in step a is paraxylene；It is mixed described in step a pair
Conjunction object is heated to be to be heated 2~3 hours under the conditions of 130~135 DEG C.
Further, the mass fraction of ultra-high molecular weight polyethylene is in super high molecular polyethylene solution obtained by step a
0.02%~0.04%.
Further, silicon wafer described in step b is P100；It is described that oxidation processes detailed process is carried out to silicon wafer are as follows: by silicon
Piece aoxidizes 1 hour under ultraviolet light irradiation；The silicon wafer for being placed in spin coating instrument is heated are as follows: by silicon wafer be heated to 50~80 DEG C,
And 3~5min is kept the temperature under this condition.
Further, when High molecular weight polyethylene solution described in step c carries out spin coating, the revolving speed of spin coating instrument be 4000rpm,
Spin-coating time is 30s.
Further, the solvent that poly- (3- hexyl thiophene) is dissolved described in step d is paraxylene, chloroform or chlorobenzene；It is described
The mixed solution of poly- (3- hexyl thiophene) and solvent is heated are as follows: 5 hours are heated under the conditions of 40~70 DEG C (to diformazan
When benzene or chlorobenzene are solvent, heated 5 hours under the conditions of 70 DEG C；It when using chloroform as solvent, is heated 5 hours under the conditions of 40 DEG C).
Further, the mass fraction of poly- (3- hexyl thiophene) is in poly- (3- hexyl thiophene) solution obtained by step d
0.001%~0.005%.
Further, the weight average molecular weight of the ultra-high molecular weight polyethylene is 3 × 106G/mol~4 × 106g/mol。
A kind of poly- (3- hexyl thiophene) conductive network structure prepared using the above method.
I.e. the invention firstly uses solvents to dissolve a certain amount of ultra-high molecular weight polyethylene, makes it in a heated condition completely
Dissolution, obtains super high molecular polyethylene solution after dissolution, at the same to silicon wafer carry out oxidation processes, oxidation is placed on rotation
Tu Yizhong and to silicon wafer heating and thermal insulation；Then obtained super high molecular polyethylene solution is placed in spin coating instrument after heating
Silicon wafer on, then with spin coating instrument carry out spin coating, after the completion of spin coating, be cooled to room temperature and obtain ultra-high molecular weight polyethylene shish-
Kebab network structure；Then poly- (3- hexyl thiophene) dissolve in a solvent, heating be formulated as poly- (3- hexyl thiophene) solution, will
The solution drop coating due to polyethylene (110) crystal face and is gathered on ultra-high molecular weight polyethylene shish-kebab network structure surface
(3- hexyl thiophene) (100) crystal face cell parameter matches very much, so P3HT can be in ultra-high molecular weight polyethylene network structure
Nucleation, and since intermolecular stronger π-π interacts, there is growth of the P3HT nanofiber on pi-pi accumulation direction excellent
Gesture, so P3HT crystal takes edge-on to be orientated, i.e., a axis is parallel to substrate (note: P3HT side group perpendicular to substrate, b axis and c-axis
Along a axis direction, pi-pi accumulation is along b axis direction, and main chain is along c-axis direction.), in addition can also be arranged along side group direction to be formed it is more
Layer structure.
Compared with prior art, the present invention has following positive beneficial effect
The present invention induces poly- (3- hexyl thiophene) epitaxial crystallization system by using the ultra-high molecular weight polyethylene of stable structure
Standby to obtain conductive network structure, this method is easy to operate, preparation time is short, and obtained P3HT conductive network structural conductive
It can be excellent；
Poly- (3- hexyl thiophene) nanofiber of edge-on orientation is obtained by this method, can intuitively be observed poly-
(3- hexyl thiophene) fiber vertical distribution is on ultra-high molecular weight polyethylene reticular structure；It is taken on P3HT nanofiber is microcosmic
Edge-on orientation, is arranged vertically in ultra-high molecular weight polyethylene network structure, forms shish-kebab structure, and macroscopical
On be isotropic, and by ultra-high molecular weight polyethylene network structure, each P3HT crystal (P3HT nanofiber) phase
Network structure is mutually contacted and is formed, and P3HT crystal (P3HT nanofiber) and silicon wafer directly contact, these structures can
The electric conductivity of P3HT network structure is remarkably reinforced；Using method of the present invention, then by control solvent type, temperature and
Mass fraction etc. is the nucleation and growth of controllable P3HT, conductive network structure required for obtaining.It is prepared by this method
P3HT conductive network structure has good electric conductivity, can be used in the preparation of conductive devices, has a good application prospect.
Detailed description of the invention
Fig. 1 shows the electric conductivity testing result figures that product is prepared in embodiment 1；The right picture is left side picture in Fig. 1
Partial enlarged view；Pure white region is the silicon wafer of bottom in figure, and ash, black network are ultra-high molecular weight polyethylene induction in figure
The conductive network that P3HT epitaxial crystallization is formed, since color is deeper in figure, more the better (figure of the partially electronically conductive performance for being partial to black
In 1 the right picture current scale known to: with the intensification of color, electric conductivity is gradually increased), thus formed P3HT network
The electric conductivity of structure is much better than silicon wafer, i.e. P3HT conductive network structure has good electric conductivity.
The figure be prepared using atomic force microscope PeakForce-TUNA Mode scans embodiment 1 it is poly- (3- oneself
Base thiophene) conductive network structure sample, apply the electrically conductive signal that the voltage of 6V obtains；
Fig. 2 indicates the height map of ultra-high molecular weight polyethylene shish-kebab network structure prepared by embodiment 1；
Fig. 3 indicates the height map of the conductive network structure of poly- (3- hexyl thiophene) prepared by embodiment 1 (by the perpendicular of figure right side
Known to straight label: white be silicon wafer, conductive network structure height be 0nm；With coloured part be conductive network structure and
With the intensification of color, the height of conductive network structure is gradually increased.)；The right picture is the partial enlargement of left side picture in Fig. 3
Figure；
Fig. 4 indicates the electric conductivity testing result figure that product is prepared in embodiment 2；The right picture is left side picture in Fig. 4
Partial enlarged view；Pure white region is the silicon wafer of bottom in figure, and ash, black network are ultra-high molecular weight polyethylene induction in figure
The conductive network that P3HT epitaxial crystallization is formed, since color is deeper in figure, more the better (figure of the partially electronically conductive performance for being partial to black
In 4 the right pictures current scale known to: with the intensification of color, electric conductivity is gradually increased), thus formed P3HT network
The electric conductivity of structure is much better than silicon wafer, i.e. P3HT conductive network structure has good electric conductivity.
The figure be prepared using atomic force microscope PeakForce-TUNA Mode scans embodiment 2 it is poly- (3- oneself
Base thiophene) conductive network structure sample, apply the electrically conductive signal that the voltage of 6V obtains；
Fig. 5 is the height map of ultra-high molecular weight polyethylene shish-kebab network structure prepared by embodiment 2；
Fig. 6 is the height map of the conductive network structure of poly- (3- hexyl thiophene) prepared by embodiment 2；The right picture in Fig. 6
For the partial enlarged view of left side picture；
Fig. 7 is the electric conductivity testing result figure for indicating to prepare product in embodiment 3；The right picture is left side figure in Fig. 7
The partial enlarged view of piece；Pure white region is the silicon wafer of bottom in figure, and ash, black network lure in figure for ultra-high molecular weight polyethylene
The conductive network of P3HT epitaxial crystallization formation is led, it is better more the partially electronically conductive performance for being partial to black since color is deeper in figure
(in figure known to the current scale of 7 the right pictures: with the intensification of color, electric conductivity is gradually increased), so the P3HT formed
The electric conductivity of network structure is much better than silicon wafer, i.e. P3HT conductive network structure has good electric conductivity.
The figure be prepared using atomic force microscope PeakForce-TUNA Mode scans embodiment 3 it is poly- (3- oneself
Base thiophene) conductive network structure sample, apply the electrically conductive signal that the voltage of 6V obtains；
Fig. 8 is the height map of ultra-high molecular weight polyethylene shish-kebab network structure prepared by embodiment 3；
Fig. 9 is the height map of the conductive network structure of poly- (3- hexyl thiophene) prepared by embodiment 3；The right picture in Fig. 9
For the partial enlarged view of left side picture；
Figure 10 is the height map of ultra-high molecular weight polyethylene shish-kebab network structure prepared by embodiment 4；
Figure 11 is the height map of the conductive network structure of poly- (3- hexyl thiophene) prepared by embodiment 4；The right figure in Figure 11
Piece is the partial enlarged view of left side picture；
Figure 12 is the height map of ultra-high molecular weight polyethylene shish-kebab network structure prepared by embodiment 5；In Figure 12
The right picture is the partial enlarged view of left side picture；
Figure 13 is the height map of the conductive network structure of poly- (3- hexyl thiophene) prepared by embodiment 5；The right figure in Figure 13
Piece is the partial enlarged view of left side picture.
Specific embodiment
The present invention is described in more details below by specific embodiment, but is not intended to restrict the invention
Protection scope.
The reagent used in following embodiment is that analysis is pure, spin coating instrument (Chinese Academy of Sciences Microelectronics Institute develops,
KW-4A type), silicon wafer (Zhejiang Li Jing Electro-optical Technology, INC. (US) 62 Martin Road, Concord, Massachusetts 017), ultraviolet lamp (the double-U-shaped sterilizing viltalight lamp of space flight hongda 30W)；Inspection
It surveys using atomic force microscope (Dimension Icon, Bruker, USA).
Embodiment 1
The weight average molecular weight of ultra-high molecular weight polyethylene used is (3.5 × 10 in the embodiment6G/mol), it is purchased from
HoechstAG,(Frankfurt am Main,Germany)；The number-average molecular weight of poly- (3- hexyl thiophene) used be 5.23 ×
103G/mol is purchased from (Shanghai Di Bai Biotechnology Co., Ltd).
A kind of poly- (3- hexyl thiophene) conductive network structure, electric conductivity detect as shown in Figure 1, resulting structures such as Fig. 3
It is shown；As seen from Figure 1, the P3HT network structure of preparation has good electric conductivity；
The preparation method of poly- (3- hexyl thiophene) the conductive network structure the following steps are included:
(1) preparation of ultra-high molecular weight polyethylene shish-kebab network structure
A. the ultra-high molecular weight polyethylene for taking 5mg is placed in paraxylene solvent and is mixed, then mixed solution exists
It is heated 2 hours under the conditions of 130 DEG C, after the completion of heating, the ultra-high molecular weight polyethylene in solution is completely dissolved, and then uses temperature
The solution being completely dissolved is diluted for 130 DEG C of paraxylene, obtains supra polymer in super high molecular polyethylene solution
The mass fraction of weight northylen is 0.02%；
B. P100 silicon wafer 1cm × 1cm is taken, then aoxidizes 1 hour under ultraviolet light irradiation, after the completion of oxidation, silicon wafer is set
In on spin coating instrument, then the silicon wafer being placed on spin coating instrument is heated, is heated to 70 DEG C, and keep the temperature 3min at such a temperature；
C. after the silicon wafer on spin coating instrument described in step b has been kept the temperature, taking temperature described in step a rapidly is 130 DEG C, mass fraction
It for 0.02% super high molecular polyethylene solution 0.03ml, is placed on silicon wafer, then starts spin coating instrument, in turning for 4000rpm
The lower spin coating 30s of speed；After the completion of spin coating, by the ultra-high molecular weight polyethylene being spin-coated on silicon wafer and silicon wafer be cooled to room temperature to get
To ultra-high molecular weight polyethylene shish-kebab network structure；Then poly- to gained super high molecular weight using atomic force microscope
Ethylene shish-kebab network structure is detected, as a result as shown in Figure 2；
(2) (ultra-high molecular weight polyethylene induces poly- (3- hexyl thiophene for the preparation of poly- (3- hexyl thiophene) conductive network structure
Pheno) epitaxial crystallization prepares conductive network structure):
D. it takes poly- (3- hexyl thiophene) 10mg to be placed in paraxylene and carries out mixed dissolution, and heat 5 under the conditions of 70 DEG C
Hour makes that poly- (3- hexyl thiophene) is taken to be completely dissolved, and obtains poly- (3- hexyl thiophene) solution that mass fraction is 0.5%；Then it adopts
0.5% poly- (3- hexyl thiophene) solution is diluted with the paraxylene solvent that temperature is 70 DEG C, obtains poly- (3- hexyl thiophene
Pheno) mass fraction be 0.005% poly- (3- hexyl thiophene) solution；
E. to take temperature obtained by step d be 70 DEG C, poly- (3- hexyl thiophene) the solution 0.03ml that mass fraction is 0.005%,
Drop coating is in ultra-high molecular weight polyethylene shish-kebab network structure prepared by step (1), after the completion of drop coating, natural cooling
It is volatilized completely to room temperature, solvent to get the conductive network structure of poly- (3- hexyl thiophene) is arrived；Then atomic force microscope pair is used
The conductive network structure for obtaining poly- (3- hexyl thiophene) is detected, as a result as shown in Figure 3.
Embodiment 2
The weight average molecular weight of ultra-high molecular weight polyethylene used is (3.5 × 10 in the embodiment6G/mol), it is purchased from
HoechstAG,(Frankfurt am Main,Germany)；The number-average molecular weight of poly- (3- hexyl thiophene) used is 5.23 ×
103G/mol is purchased from (Shanghai Di Bai Biotechnology Co., Ltd).
A kind of poly- (3- hexyl thiophene) conductive network structure, electric conductivity detect as shown in figure 4, resulting structures such as Fig. 6
It is shown；As seen from Figure 4, the P3HT network structure of preparation has good electric conductivity；
The preparation method of poly- (3- hexyl thiophene) the conductive network structure the following steps are included:
(1) preparation of ultra-high molecular weight polyethylene shish-kebab network structure
A. the ultra-high molecular weight polyethylene for taking 5mg is placed in paraxylene solvent and is mixed, then mixed solution exists
It is heated 2 hours under the conditions of 130 DEG C, after the completion of heating, the ultra-high molecular weight polyethylene in solution is completely dissolved, and then uses temperature
The solution being completely dissolved is diluted for 130 DEG C of paraxylene, obtains supra polymer in super high molecular polyethylene solution
The mass fraction of weight northylen is 0.03%；
B. P100 silicon wafer 1cm × 1cm is taken, then aoxidizes 1 hour under ultraviolet light irradiation, after the completion of oxidation, silicon wafer is set
In on spin coating instrument, then the silicon wafer being placed on spin coating instrument is heated, is heated to 70 DEG C, and keep the temperature 3min at such a temperature；
C. after the silicon wafer on spin coating instrument described in step b has been kept the temperature, taking temperature described in step a rapidly is 130 DEG C, mass fraction
It for 0.03% super high molecular polyethylene solution 0.03ml, is placed on silicon wafer, then starts spin coating instrument, in turning for 4000rpm
The lower spin coating 30s of speed；After the completion of spin coating, by the ultra-high molecular weight polyethylene being spin-coated on silicon wafer and silicon wafer be cooled to room temperature to get
To ultra-high molecular weight polyethylene shish-kebab network structure；Then poly- to super high molecular weight is obtained using atomic force microscope
Ethylene shish-kebab network structure is detected, as a result as shown in Figure 5；
(2) (ultra-high molecular weight polyethylene induces poly- (3- hexyl thiophene for the preparation of poly- (3- hexyl thiophene) conductive network structure
Pheno) epitaxial crystallization prepares conductive network structure):
D. it takes poly- (3- hexyl thiophene) 10mg to be placed in paraxylene and carries out mixed dissolution, and heat 5 under the conditions of 70 DEG C
Hour makes that poly- (3- hexyl thiophene) is taken to be completely dissolved, and obtains poly- (3- hexyl thiophene) solution that mass fraction is 0.5%；Then it adopts
0.5% poly- (3- hexyl thiophene) solution is diluted to poly- (3- hexyl thiophene) quality with the paraxylene solvent that temperature is 70 DEG C
Poly- (3- hexyl thiophene) solution that score is 0.005%；
E. to take temperature obtained by step d be 70 DEG C, poly- (3- hexyl thiophene) the solution 0.03ml that mass fraction is 0.005%,
Drop coating is in ultra-high molecular weight polyethylene shish-kebab network structure prepared by step (1), after the completion of drop coating, natural cooling
It is volatilized completely to room temperature, solvent to get the conductive network structure of poly- (3- hexyl thiophene) is arrived；Then atomic force microscope pair is used
The conductive network structure for obtaining poly- (3- hexyl thiophene) is detected, as a result as shown in Figure 6.
Embodiment 3
The molecular weight of ultra-high molecular weight polyethylene used is (3.5 × 10 in the embodiment6It g/mol), is weight average molecular weight,
Purchased from HoechstAG, (Frankfurt am Main, Germany)；The number-average molecular weight of poly- (3- hexyl thiophene) used is
5.23×103G/mol is purchased from (Shanghai Di Bai Biotechnology Co., Ltd).
A kind of poly- (3- hexyl thiophene) conductive network structure, electric conductivity detect as shown in fig. 7, resulting structures such as Fig. 9
It is shown；As seen from Figure 7, the P3HT network structure of preparation has good electric conductivity；
The preparation method of poly- (3- hexyl thiophene) the conductive network structure the following steps are included:
(1) preparation of ultra-high molecular weight polyethylene shish-kebab network structure
A. the ultra-high molecular weight polyethylene for taking 10mg is placed in paraxylene solvent and is mixed, then by mixed solution
It is heated 2 hours under the conditions of 130 DEG C, after the completion of heating, the ultra-high molecular weight polyethylene in solution is completely dissolved, then using temperature
Degree is diluted the solution being completely dissolved for 130 DEG C of paraxylene, obtains superelevation point in super high molecular polyethylene solution
The mass fraction of sub- weight northylen is 0.04%；
B. P100 silicon wafer 1cm × 1cm is taken, then aoxidizes 1 hour under ultraviolet light irradiation, after the completion of oxidation, silicon wafer is set
In on spin coating instrument, then the silicon wafer being placed on spin coating instrument is heated, is heated to 70 DEG C, and keep the temperature 3min at such a temperature；
C. after the silicon wafer on spin coating instrument described in step b has been kept the temperature, taking temperature described in step a rapidly is 130 DEG C, mass fraction
It for 0.04% super high molecular polyethylene solution 0.03ml, is placed on silicon wafer, then starts spin coating instrument, in turning for 4000rpm
The lower spin coating 30s of speed；After the completion of spin coating, by the ultra-high molecular weight polyethylene being spin-coated on silicon wafer and silicon wafer be cooled to room temperature to get
To ultra-high molecular weight polyethylene shish-kebab network structure；Then using atomic force microscope to obtained super high molecular weight
Polyethylene shish-kebab network structure is detected, as a result as shown in Figure 8；
(2) (ultra-high molecular weight polyethylene induces poly- (3- hexyl thiophene for the preparation of poly- (3- hexyl thiophene) conductive network structure
Pheno) epitaxial crystallization prepares conductive network structure):
D. it takes poly- (3- hexyl thiophene) 10mg to be placed in chloroform and carries out mixed dissolution, and heated 5 hours under the conditions of 40 DEG C
Make that poly- (3- hexyl thiophene) is taken to be completely dissolved, obtains poly- (3- hexyl thiophene) solution that mass fraction is 0.5%；Then using temperature
0.5% poly- (3- hexyl thiophene) solution is diluted to poly- (3- hexyl thiophene) mass fraction for 40 DEG C of chloroform solvent by degree
0.005% poly- (3- hexyl thiophene) solution；
Ultra-high molecular weight polyethylene shish-kebab network structure prepared by step (1) is heated to 40 DEG C by e, takes step d
Poly- (3- hexyl thiophene) the solution 0.03ml that gained temperature is 40 DEG C, mass fraction is 0.005%, drop coating are being heated to 40 DEG C
In ultra-high molecular weight polyethylene shish-kebab network structure, after the completion of drop coating, cooled to room temperature, solvent volatilize completely,
Obtain the conductive network structure of poly- (3- hexyl thiophene)；Then using atomic force microscope to obtained poly- (3- hexyl thiophene)
Conductive network structure detected, as a result as shown in Figure 9.
Embodiment 4
The molecular weight of ultra-high molecular weight polyethylene used is (3.5 × 10 in the embodiment6It g/mol), is weight average molecular weight,
Purchased from HoechstAG, (Frankfurt am Main, Germany)；The number-average molecular weight of poly- (3- hexyl thiophene) used is
36.6×103G/mol is purchased from (1-Material Inc.).
A kind of poly- (3- hexyl thiophene) conductive network structure, resulting structures are as shown in figure 11.
The preparation method of poly- (3- hexyl thiophene) the conductive network structure the following steps are included:
(1) preparation of ultra-high molecular weight polyethylene shish-kebab network structure
A. the ultra-high molecular weight polyethylene for taking 5mg is placed in paraxylene solvent and is mixed, and then polyhybird solution exists
It is heated 2 hours under the conditions of 130 DEG C, after the completion of heating, the ultra-high molecular weight polyethylene in solution is completely dissolved, and then uses temperature
The solution being completely dissolved is diluted for 130 DEG C of paraxylene, obtains supra polymer in super high molecular polyethylene solution
The mass fraction of weight northylen is 0.02%；
B. P100 silicon wafer 1cm × 1cm is taken, then aoxidizes 1 hour under ultraviolet light irradiation, after the completion of oxidation, silicon wafer is set
In on spin coating instrument, then the silicon wafer being placed on spin coating instrument is heated, is heated to 70 DEG C, and keep the temperature 3min at such a temperature；
C. after the silicon wafer on spin coating instrument described in step b has been kept the temperature, taking temperature described in step a rapidly is 130 DEG C, mass fraction
It for 0.02% super high molecular polyethylene solution 0.03ml, is placed on silicon wafer, then starts spin coating instrument, in turning for 4000rpm
The lower spin coating 30s of speed；After the completion of spin coating, by the ultra-high molecular weight polyethylene being spin-coated on silicon wafer and silicon wafer be cooled to room temperature to get
To ultra-high molecular weight polyethylene shish-kebab network structure；Then using atomic force microscope to obtained super high molecular weight
Polyethylene shish-kebab network structure is detected, and the results are shown in Figure 10；
(2) (ultra-high molecular weight polyethylene induces poly- (3- hexyl thiophene for the preparation of poly- (3- hexyl thiophene) conductive network structure
Pheno) epitaxial crystallization prepares conductive network structure):
D. it takes poly- (3- hexyl thiophene) 10mg to be placed in chlorobenzene and carries out mixed dissolution, and heated 5 hours under the conditions of 70 DEG C
Make that poly- (3- hexyl thiophene) is taken to be completely dissolved, obtains poly- (3- hexyl thiophene) solution that mass fraction is 0.5%；Then using temperature
0.5% poly- (3- hexyl thiophene) solution is diluted to poly- (3- hexyl thiophene) mass fraction for 70 DEG C of chlorobenzene solvent by degree
0.005% poly- (3- hexyl thiophene) solution；
E. ultra-high molecular weight polyethylene shish-kebab network structure prepared by step (1) is heated to 70 DEG C, takes step
Temperature obtained by d is 70 DEG C, poly- (3- hexyl thiophene) the solution 0.03ml that mass fraction is 0.005%, and drop coating is being heated to 70 DEG C
Ultra-high molecular weight polyethylene shish-kebab network structure on, after the completion of drop coating, cooled to room temperature, solvent are waved completely
It sends out to get the conductive network structure of poly- (3- hexyl thiophene) is arrived；Then using atomic force microscope to obtained poly- (3- hexyl thiophene
Pheno) conductive network structure detected, as a result as shown in figure 11.
Embodiment 5
The molecular weight of ultra-high molecular weight polyethylene used is (3.5 × 10 in the embodiment6It g/mol), is weight average molecular weight,
Purchased from HoechstAG, (Frankfurt am Main, Germany)；The number-average molecular weight of poly- (3- hexyl thiophene) used is
5.23×103G/mol is purchased from (Shanghai Di Bai Biotechnology Co., Ltd).
A kind of poly- (3- hexyl thiophene) conductive network structure, resulting structures are as shown in figure 13.
The preparation method of poly- (3- hexyl thiophene) the conductive network structure the following steps are included:
(1) preparation of ultra-high molecular weight polyethylene shish-kebab network structure
A. the ultra-high molecular weight polyethylene for taking 5mg is placed in paraxylene solvent and is mixed, and then polyhybird solution exists
It is heated 2 hours under the conditions of 130 DEG C, after the completion of heating, the ultra-high molecular weight polyethylene in solution is completely dissolved, and then uses temperature
The solution being completely dissolved is diluted for 130 DEG C of paraxylene, obtains supra polymer in super high molecular polyethylene solution
The mass fraction of weight northylen is 0.04%；
B. P100 silicon wafer 1cm × 1cm is taken, then aoxidizes 1 hour under ultraviolet light irradiation, after the completion of oxidation, silicon wafer is set
In on spin coating instrument, then the silicon wafer being placed on spin coating instrument is heated, is heated to 70 DEG C, and keep the temperature 3min at such a temperature；
C. after the silicon wafer on spin coating instrument described in step b has been kept the temperature, taking temperature obtained by step a rapidly is 130 DEG C, mass fraction
It is placed on silicon wafer for 0.04% super high molecular polyethylene solution 0.03ml, then starts spin coating instrument, in the revolving speed of 4000rpm
Lower spin coating 30s；After the completion of spin coating, silicon wafer is cooled to room temperature to get ultra-high molecular weight polyethylene shish-kebab network knot is arrived
Structure；Then obtained ultra-high molecular weight polyethylene shish-kebab network structure is detected using atomic force microscope, is tied
Fruit is as shown in figure 12；
(2) (ultra-high molecular weight polyethylene induces poly- (3- hexyl thiophene for the preparation of poly- (3- hexyl thiophene) conductive network structure
Pheno) epitaxial crystallization prepares conductive network structure):
D. it takes poly- (3- hexyl thiophene) 10mg to be placed in paraxylene and carries out mixed dissolution, and heat 5 under the conditions of 70 DEG C
Hour makes that poly- (3- hexyl thiophene) is taken to be completely dissolved, and obtains poly- (3- hexyl thiophene) solution that mass fraction is 0.5%；Then it adopts
0.5% poly- (3- hexyl thiophene) solution is diluted to poly- (3- hexyl thiophene) quality with the paraxylene solvent that temperature is 70 DEG C
Poly- (3- hexyl thiophene) solution that score is 0.005%；
E. ultra-high molecular weight polyethylene shish-kebab network structure prepared by step (1) is heated to 70 DEG C, then taken
Temperature obtained by step d is 70 DEG C, poly- (3- hexyl thiophene) the solution 0.03ml that mass fraction is 0.005%, and drop coating is being heated to
In 70 DEG C of ultra-high molecular weight polyethylene shish-kebab network structure, after the completion of drop coating, cooled to room temperature, solvent are complete
Full volatilization is to get the conductive network structure for arriving poly- (3- hexyl thiophene)；Then using atomic force microscope to obtain it is poly- (3- oneself
Base thiophene) conductive network structure detected, as a result as shown in figure 13.
Claims (9)
1. a kind of preparation method of poly- (3- hexyl thiophene) conductive network structure, which is characterized in that method includes the following steps:
(1) preparation of ultra-high molecular weight polyethylene shish-kebab network structure
A. it takes ultra-high molecular weight polyethylene to carry out dissolution mixing in a solvent, then mixture is heated, make therein super
High molecular weight polyethylene is completely dissolved, and the solution of ultra-high molecular weight polyethylene is obtained after being completely dissolved；
B. silicon wafer is taken, oxidation processes are carried out to silicon wafer, after the completion of oxidation processes, the silicon wafer after oxidation are placed in spin coating instrument, so
The silicon wafer being placed on spin coating instrument is heated and kept the temperature afterwards；
C. after the completion of silicon wafer heating and thermal insulation described in step b, the ultra-high molecular weight polyethylene after dissolving by heating described in step a is molten
Liquid, which is placed on the silicon wafer of spin coating instrument, carries out spin coating, after the completion of spin coating, the ultra-high molecular weight polyethylene being spin-coated on silicon wafer is cooling
To room temperature to get arrive ultra-high molecular weight polyethylene shish-kebab network structure；
(2) preparation of poly- (3- hexyl thiophene) conductive network structure:
D. it takes poly- (3- hexyl thiophene) to be dissolved in solvent, then the mixed solution of poly- (3- hexyl thiophene) and solvent is heated
It is completely dissolved poly- (3- hexyl thiophene), the solution of poly- (3- hexyl thiophene) is obtained after dissolution；
E. the super high molecular weight poly- (3- hexyl thiophene) the solution drop coating that step d is prepared being prepared in step (1) is poly-
In ethylene shish-kebab network structure；It after the completion of drop coating, volatilizees naturally, solvent obtains poly- (3- hexyl thiophene after volatilizing completely
Pheno) conductive network structure；
Or the ultra-high molecular weight polyethylene shish-kebab being cooled to room temperature on the silicon wafer that step (1) is prepared first
Network structure is heated, and is heated to that temperature is identical as poly- (3- hexyl thiophene) temperature of solution obtained by step d, and heating is completed
Afterwards, it keeps the temperature at such a temperature；After the completion of heat preservation, then by poly- (3- hexyl thiophene) solution drop coating silicon wafer after heat preservation obtained by step d
On ultra-high molecular weight polyethylene shish-kebab network structure on；After the completion of drop coating, volatilize naturally, after solvent volatilizees completely
Obtain the conductive network structure of poly- (3- hexyl thiophene).
2. the preparation method of poly- (3- hexyl thiophene) conductive network structure according to claim 1, which is characterized in that step
The solvent that ultra-high molecular weight polyethylene is dissolved described in a is paraxylene；Mixture is heated to be in 130~135 DEG C of conditions
Lower heating 2~3 hours.
3. the preparation method of poly- (3- hexyl thiophene) conductive network structure according to claim 2, which is characterized in that step
The mass fraction of super high molecular polyethylene solution obtained by a is 0.02%~0.04%.
4. the preparation method of poly- (3- hexyl thiophene) conductive network structure according to claim 1, which is characterized in that step
Silicon wafer described in b is P100 silicon wafer；The detailed process of oxidation processes is carried out to silicon wafer are as follows: aoxidize silicon wafer under ultraviolet light irradiation
1 hour；The silicon wafer for being placed in spin coating instrument is heated are as follows: by silicon wafer be heated to 50~80 DEG C and under this condition heat preservation 3~
5min。
5. the preparation method of poly- (3- hexyl thiophene) conductive network structure according to claim 1, which is characterized in that step
When super high molecular polyethylene solution described in c carries out spin coating, the revolving speed of spin coating instrument is 4000rpm, and the time of spin coating is 30s.
6. the preparation method of poly- (3- hexyl thiophene) conductive network structure according to claim 1, which is characterized in that step
The solvent that poly- (3- hexyl thiophene) is dissolved described in d is paraxylene, chloroform or chlorobenzene；Described pair poly- (3- hexyl thiophene) and solvent
Mixed solution be heated to be and heated 5 hours under the conditions of 40~70 DEG C.
7. the preparation method of poly- (3- hexyl thiophene) conductive network structure according to claim 6, which is characterized in that step
The mass fraction of poly- (3- hexyl thiophene) is 0.001%~0.005% in poly- (3- hexyl thiophene) solution obtained by d.
8. the preparation method of described in any item poly- (3- hexyl thiophene) conductive network structures according to claim 1~7, feature
It is, the weight average molecular weight of the ultra-high molecular weight polyethylene is 3 × 106G/mol~4 × 106g/mol。
9. a kind of poly- (3- hexyl thiophene) conductive network structure being prepared using method described in claim 1.
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